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Hach DR/850 Procedures Manual Download Page 4

4

TABLE OF CONTENTS,

continued

Distillation ............................................................................................................................. 55

SECTION 3 WASTE MANAGEMENT AND SAFETY....................................................... 57

Waste Management................................................................................................................ 57

Waste Minimization ........................................................................................................  57
Regulatory Overview ......................................................................................................  57
Hazardous Waste Definition............................................................................................  58
Characteristic Hazardous Waste Codes...........................................................................  59
How to Determine if Waste is Hazardous .......................................................................  59
Examples of Hazardous Waste ........................................................................................  60
Hazardous Waste Disposal ..............................................................................................  60
Management of Specific Wastes .....................................................................................  61
Resources ........................................................................................................................  62

Material Safety Data Sheets................................................................................................... 63

How to Obtain an MSDS ................................................................................................ 63
Sections of the MSDS ..................................................................................................... 63

Safety ..................................................................................................................................... 66

Material Safety Data Sheet..............................................................................................  66
Reading Labels Carefully................................................................................................  66
Protective Equipment ......................................................................................................  66
First Aid Equipment and Supplies ..................................................................................  67
General Safety Rules .......................................................................................................  67
OSHA Chemical Hygiene Plan .......................................................................................  68

SECTION 4 PROCEDURES.................................................................................................. 69

ALUMINUM, Aluminon Method .......................................................................................... 71

BROMINE, DPD Method....................................................................................................... 77

CHLORAMINE, MONO, Low Range, CHLORAMINE, MONO, High Range, Indophenol

Method ............................................................................................................................. 93

CHLORINE, FREE, Ultra-high Range, DPD Method ......................................................... 101

CHLORINE, TOTAL, Ultra-High Range, DPD Method ..................................................... 109

CHLORINE, FREE, DPD Method ....................................................................................... 117

CHLORINE, TOTAL, DPD Method .................................................................................... 125

CHLORINE, FREE, DPD Test ‘N Tube™ Method ............................................................. 133

CHLORINE, TOTAL, DPD Test ‘N Tube™ Method .......................................................... 141

CHLORINE DIOXIDE, DPD Method ................................................................................. 147

CYANIDE, Pyridine-Pyrazalone Method............................................................................. 155

CYANURIC ACID, Turbidimetric Method.......................................................................... 165

FLUORIDE, SPADNS Method ............................................................................................ 169

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Summary of Contents for DR/850

Page 1: ...48450 22 DR 850 COLORIMETER PROCEDURES MANUAL Hach Company 1997 2007 2013 All rights reserved Printed in the U S A te dk 03 13 7ed...

Page 2: ...2...

Page 3: ...g Sample Cells 31 Using AccuVac Ampuls 32 Using Reagent Powder Pillows 33 Using PermaChem Pillows 33 Reagent and Standard Stability 34 Interferences 34 pH Interference 35 Accuracy and Precision 36 Sta...

Page 4: ...Data Sheet 66 Reading Labels Carefully 66 Protective Equipment 66 First Aid Equipment and Supplies 67 General Safety Rules 67 OSHA Chemical Hygiene Plan 68 SECTION 4 PROCEDURES 69 ALUMINUM Aluminon Me...

Page 5: ...N Tube Titanium Trichloride Reduction Method 277 OXYGEN DEMAND CHEMICAL Manganese III Digestion Method 285 ORGANIC CARBON TOTAL Low Range Direct Method 291 ORGANIC CARBON TOTAL Mid Range Direct Metho...

Page 6: ...Methylene Blue Method 413 SURFACTANTS ANIONIC Also called Detergents Crystal Violet Method 417 SUSPENDED SOLIDS Photometric Method 421 TANNIN AND LIGNIN Tyrosine Method 425 TOXTRAK TOXICITY TEST Color...

Page 7: ...on on waste management regulations waste disposal and resources on waste management The Safety portion covers reading an MSDS and general safety guidelines Section 4 Procedures Section 4 contains step...

Page 8: ...8...

Page 9: ...9 Sample Procedure Explained...

Page 10: ...10 Sample Procedure Explained continued...

Page 11: ...11 Sample Procedure Explained continued...

Page 12: ...12 Sample Procedure Explained continued...

Page 13: ...s the standard reference work for water analysis Many procedures contained in this manual are based on Standard Methods g L micrograms per liter ppb AV AccuVac mL milliliter approximately the same as...

Page 14: ...3 15 mg L Cr6 mg L CrO4 2 2 231 mg L Cr6 mg L Na2CrO4 3 115 mg L Mg CaCO3 mg L Mg 0 2428 mg L Mn mg L KMnO4 2 876 mg L Mn mg L MnO4 2 165 mg L Mo6 mg L MoO4 2 1 667 mg L Mo6 mg L Na2MoO4 2 146 mg L N...

Page 15: ...00 CaCO3 German Parts 100 000 CaO meq L1 g L CaO lbs cu ft CaCO3 mg L CaCO3 1 0 0 07 0 058 0 1 0 056 0 02 5 6x10 4 6 23x10 5 English gr gal CaCO3 14 3 1 0 0 83 1 43 0 83 0 286 8 0x10 3 8 9x10 4 US gr...

Page 16: ...12 9 12 4 12 0 11 5 11 1 39 2 4 13 4 13 2 13 0 12 5 12 1 11 7 11 2 10 8 41 0 5 13 1 12 8 12 6 12 2 11 8 11 4 10 9 10 5 42 8 6 12 7 12 5 12 3 11 9 11 5 11 1 10 7 10 3 44 6 7 12 4 12 2 12 0 11 6 11 2 10...

Page 17: ...8 6 37 7 0 6 8 6 7 6 5 6 3 6 0 5 8 5 6 100 4 38 6 9 6 7 6 6 6 4 6 2 5 9 5 7 5 5 102 2 39 6 8 6 6 6 5 6 3 6 1 5 8 5 6 5 4 104 0 40 6 7 6 5 6 4 6 2 6 0 5 7 5 5 5 3 105 8 41 6 6 6 4 6 3 6 1 5 9 5 6 5 4 5...

Page 18: ...ses may change the amount of a chemical species available for analysis Normally analyze the samples as soon as possible after collection especially when the analyte concentration is expected to be low...

Page 19: ...48 hours 23 24 Cyanide total and amenable to chlorination P G Cool 4 C NaOH to pH 12 0 6 g ascorbic acid6 14 days7 25 Fluoride P None required 28 days 27 Hardness P G HNO3 to pH 2 H2SO4 to pH 2 6 mon...

Page 20: ...apply to the following materials Hydrochloric acid HCl in water solutions at concentrations of 0 04 by weight or less pH about 1 96 or greater Nitric acid HNO3 in water solutions at concentrations of...

Page 21: ...samples from wells after the pump has run long enough to deliver water representative of the ground water feeding the well It is hard to obtain a truly representative sample when collecting surface w...

Page 22: ...assware with deionized water For ammonia and Kjeldahl nitrogen rinse with ammonia free water Correcting for Volume Additions If you use a large volume of preservative correct for the volume of preserv...

Page 23: ...tration uses a medium usually filter paper to retain particles but pass solution This is especially helpful when sample turbidity interferes with analysis Two general methods of filtration are gravity...

Page 24: ...paratus at the end of a procedure Gravity filtration is better for retaining fine particles For faster filtering add solution until the filter paper cone is three fourths filled Never fill the cone co...

Page 25: ...le easily pipet the chosen sample portion into a clean graduated cylinder or volumetric flask for more accurate work Fill the cylinder or flask to the desired volume with deionized water Mix well Use...

Page 26: ...d with an equal volume of water what is the level at which copper will not interfere The level at which copper will not interfere in the undiluted sample is at or below 200 mg L Using Pipets and Gradu...

Page 27: ...ed mark If the serological pipet has marks extended to the tip of the pipet fill the pipet to the desired volume and drain all the sample from the pipet Then blow the sample out of the pipet tip for a...

Page 28: ...olution could leak into the pipet and cause corrosion Operating the TenSette Pipet 1 Attach a clean tip by holding the pipet body in one hand and gently pressing the large end of the pipet tip onto th...

Page 29: ...ixing sample in a round sample cell or mixing cylinder invert the cell or cylinder see Figure 4 Hold the cell in a vertical position with the cap on top Invert the cell so the cap is on the bottom Ret...

Page 30: ...30 CHEMICAL ANALYSIS INFORMATION continued Figure 4 Inverting a Sample Cell Figure 5 Swirling a Graduated Cylinder...

Page 31: ...extended periods of time Finish the cleaning procedure with a few rinses of deionized water and allow to dry Individual procedures often recommend specific cleaning methods Cleaning Sample Cells Most...

Page 32: ...3 Transfer 10 mL to another sample cell use fill mark for analysis Using AccuVac Ampuls AccuVac ampuls contain pre measured powder or liquid in optical quality glass ampuls 1 Collect the sample in a b...

Page 33: ...test Open the poly powder pillows with nail clippers or scissors see Figure 7 Figure 7 Opening Powder Pillows Using PermaChem Pillows 1 Tap the pillow on a hard surface to collect the powdered reagent...

Page 34: ...e reagent shelf life run a standard to check its effectiveness Interferences Substances in the sample may interfere with a measurement Hach mentions common interferences in the test procedures The rea...

Page 35: ...sequences etc may be ignored Mix well 3 Measure the pH of the reagent blank with a pH meter 4 Compare the pH values of your analyzed sample with the reagent blank 5 If there is little difference in th...

Page 36: ...led instructions given If you get about 100 recovery for each addition everything is working right and your results are correct If you don t get about 100 recovery for each addition a problem exists Y...

Page 37: ...increase A possible cause could be interferences Other causes include defective reagents incorrect technique a defective instrument apparatus or defective standard used for the standard addition If i...

Page 38: ...ents Use Correct Procedure and Repeat B Are Interferences Present Analysis Is Correct Analysis Is Incorrect Analysis May be Correct Do Multiple Standard Additions On Sample Give Uniform Increments Is...

Page 39: ...esult if the increases are uniform Suppose the sample result for iron was 1 0 mg L Because interferences may be present a standard addition of 0 1 mL of a 50 mg L iron standard to a 25 mL sample is ma...

Page 40: ...dure reagents or instrument It is recommended Branch B be performed to verify the supposed interference The plot for sample B shows a common chemical interference which becomes less or even zero as th...

Page 41: ...41 CHEMICAL ANALYSIS INFORMATION continued Figure 10 Multiple Standard Additions Graph...

Page 42: ...uch closer to the correct result 0 8 mg L Apparent interferences may also be caused by a defect in the instrument or standards Before assuming the interference is chemical check Branch B Example D The...

Page 43: ...sent proceed to Branch C If they are not present the analysis is correct If you still cannot identify the problem extra help is available Please call our Technical Support Group at 800 227 4224 U S A...

Page 44: ...ion The USEPA defines the method detection limit MDL as the minimum concentration that can be determined with 99 confidence that the true concentration is greater than zero Since the MDL will vary fro...

Page 45: ...on standard in iron free deionized water Eight portions of the standard were tested according to the FerroZine method with the following results Using a calculator program the average concentration 0...

Page 46: ...ertainty in chemical measurements may be due to systematic errors and or random errors A systematic error is a mistake that is always the same for every measurement made For example a blank can add to...

Page 47: ...he blank value will be subtracted from each reading Repeat the reagent blank adjust for each new lot of reagents Note After entering a reagent blank adjust the display may flash limit when zeroing if...

Page 48: ...an adjustment factor The factor is the same for all concentrations The instrument will remember the factor indefinitely and will display the standard adjustment icon when it is used Adjust the calibr...

Page 49: ...test Run tests as described in the procedure on each prepared standard Pour the customary volume of each known solution into a separate clean sample cell of the type specified for your instrument 2 St...

Page 50: ...olumns The T Ten value is the first number of the T reading and the T Units value is the second number of the T reading For example if the instrument reading was 46 the 40 line in the T Tens column an...

Page 51: ...slope and the y intercept USEPA Approved and Accepted Definitions The United States Environmental Protection Agency USEPA establishes limits for maximum contamination levels of certain constituents i...

Page 52: ...and compiled in the Code of Federal Regulations USEPA approved methods may be used for reporting results to the USEPA and other regulatory agencies USEPA Accepted Hach has developed several procedures...

Page 53: ...d TKN EPA Mild Digestion with Hot Plate for Metals Analysis Only 1 Acidify the entire sample at the time of collection with concentrated nitric acid by adding 5 mL of acid per liter or quart of sample...

Page 54: ...light in color or does not change color or appearance with continued refluxing 6 Again evaporate to near dryness do not bake and cool the beaker If any residue or precipitate results from the evapora...

Page 55: ...form of the sample and are found in the Digesdahl Digestion Apparatus Instruction Manual which is included with each Digesdahl Digestion Apparatus Distillation Distillation is an effective way of sep...

Page 56: ...56 SAMPLE PRETREATMENT continued Figure 12 General Purpose Distillation Apparatus with Heater and Support Apparatus...

Page 57: ...possible Buy chemicals in small quantities which will be used before they expire This eliminates disposal of outdated materials Clean glassware and laboratory apparatus with non hazardous soaps when p...

Page 58: ...ulate additional materials as hazardous waste Be aware that many very toxic compounds are not regulated by this definition of hazardous waste However improper management or disposal of these compounds...

Page 59: ...S is enough to decide If the product is specifically listed in the regulation it is a hazardous waste You also need to decide if it has any characteristics of a hazardous waste Physical information on...

Page 60: ...sts to determine if the final material is a hazardous waste Examples of tests using Hach reagents that generate hazardous waste include those containing mercury or mercury compounds such as COD tests...

Page 61: ...sal Hazardous or contact state and local regulators for assistance Management of Specific Wastes Hach has several documents to assist customers in managing waste generated from our products You can ob...

Page 62: ...the Resource Conservation and Recovery Act RCRA The RCRA Hotline number is 1 800 424 9346 You may also get a copy of the appropriate regulations Federal hazardous waste regulations are found in 40 CFR...

Page 63: ...r Small Business U S Government Printing Office Washington DC 1986 Material Safety Data Sheets Material safety data sheets MSDS describe the hazards of chemical products This section describes the inf...

Page 64: ...listed in SARA 313 If the component is listed and you use more than the amount listed you must report this to the USEPA every year TLV Threshold Limit Value The maximum airborne concentration for an 8...

Page 65: ...ity yellow and special hazards white 5 Health Hazard Data This section describes different ways the chemical can enter your body ingestion inhalation skin contact It also gives acute immediate and chr...

Page 66: ...fety information about the products Always read the MSDS before using a new product Reading Labels Carefully Read each reagent label carefully Pay particular attention to the precautions given Never r...

Page 67: ...ions For field work carry a portable eyewash unit Laboratories should also have appropriate fire extinguishers and fume hoods General Safety Rules Follow these rules to make work with toxic and hazard...

Page 68: ...th Administration OSHA enforces laws about the control exposure to hazardous chemicals in laboratories These regulations are in Title 29 CFR 1910 1450 They apply to all employers who use hazardous che...

Page 69: ...69 SECTION 4 PROCEDURES...

Page 70: ...70...

Page 71: ...water before use to avoid errors due to contaminants absorbed on the glass Note Sample temperature must be 20 25 C 68 77 F for accurate results 4 Add the contents of one Ascorbic Acid Powder Pillow St...

Page 72: ...place the blank into the cell holder Tightly cover the sample cell with the instrument cap 13 Press ZERO The cursor will move to the right then the display will show 0 000 mg L Al Note If Reagent Blan...

Page 73: ...entration should increase 0 1 mg L for each 0 1 mL of standard added d If these increases do not occur see Standard Additions Section 1 for more information Standard Solution Method Prepare a 0 40 mg...

Page 74: ...color changes from colorless to yellow 3 Add one drop of 5 25 N Sulfuric Acid Standard Solution to change the solution from yellow back to colorless Continue with the test Alkalinity 1000 mg L as CaCO...

Page 75: ...and the fluoride present in the sample was 1 0 mg L F the point where the 0 7 grid line intersects with the 1 0 mg L F grid line falls between the 1 2 and 1 3 mg L Al curves In this case the true alu...

Page 76: ...40 49 Sodium Hydroxide Standard Solution 5 0 N 100 mL MDB 2450 32 Sodium Hydroxide Standard Solution 5 0 N 50 mL SCDB 2450 26 Sulfuric Acid Standard Solution 5 25 N 100 mL MDB 2449 32 Water deionized...

Page 77: ...e Br2 powder pillows Press PRGM The display will show PRGM Note For most accurate results perform a Reagent Blank Correction using deionized water see Section 1 2 Press 5 ENTER The display will show m...

Page 78: ...ss TIMER ENTER A three minute reaction period will begin 8 When the timer beeps place the sample into the cell holder Tightly cover the sample cell with the instrument cap 9 Press READ The cursor will...

Page 79: ...ly and cannot be preserved for later analysis 4 Place the blank in the cell holder Tightly cover the sample cell with the instrument cap 5 Press ZERO The cursor will move to the right then the display...

Page 80: ...ensure a representative sample Let the container overflow with the sample several times then cap the sample container so there is no headspace air above the sample If sampling with a sample cell rins...

Page 81: ...sample result the calculated mg L Br2 added step e g If this increase does not occur see Standard Additions in Section 1 for more information Standard Additions Method using AccuVac Ampuls a Snap the...

Page 82: ...ined a standard deviation of 0 02 mg L bromine In a single laboratory using a standard solution of 2 31 mg L bromine and two representative lots of AccuVac Ampuls with the instrument a single operator...

Page 83: ...ate sample aliquot then add the same amount to the sample being tested Correct for volume addition See Section 1 Correcting for Volume Additions Chlorine Interferes at all levels Chlorine Dioxide Inte...

Page 84: ...olution PourRite ampule 25 30 mg L 2 mL 20 pkg 26300 20 DPD Total Chlorine Reagent SwifTest 250 Tests 28024 00 Potassium Iodide Solution 30 g L 100 mL MDB 343 32 Sodium Arsenite 5 g L 100 mL MDB 1047...

Page 85: ...older as illustrated The cell s tab should be at the 2 o clock position Make sure the sample cell tab is completely seated in the cell holder slot 5 Press ZERO The cursor will move to the right then t...

Page 86: ...esh before use 2 Add the contents of one Buffer Powder Pillow pH 8 3 to about 50 mL of organic free water in a clean 100 mL Class A volumetric flask Swirl to dissolve the powder 3 Using a Class A volu...

Page 87: ...mix thoroughly This is a nominal 4 5 mg L as Cl2 monochloramine standard Use this standard within 1 hour of preparation Method Performance Precision In a single laboratory using a monochloramine stand...

Page 88: ...50 mg L SO3 2 Tyrosine 1 mg L N Urea 10 mg L N Zinc 5 mg L Table 9 Non interfering Substances Continued Substance Maximum Level Tested Table 10 Interfering Substances Interfering Substance and its ef...

Page 89: ...to your DR 850 or DR 890 1 Turn on the instrument by pressing the ON key 2 Press the SETUP key 3 Press the down arrow key until the prompt line shows USER 4 Press the ENTER key 5 Enter 8138 followed b...

Page 90: ...0 34 0 7 0 35 63 8 0 36 57 9 0 37 199 10 0 38 104 11 0 39 62 12 64 40 74 13 176 41 61 14 120 42 45 15 106 43 1 16 0 44 204 17 0 45 0 18 0 46 5 19 0 47 10 20 67 48 1 21 108 49 44 22 50 50 0 23 0 51 0...

Page 91: ...fer Powder Pillows pH 8 3 25 pkg 898 68 Nitrogen Ammonia Standard Solution 100 mg L as NH3 N 500 mL 24065 49 Chlorine Solution Voluette Ampule 50 75 mg L 16 pkg 14268 10 OPTIONAL APPARATUS Beaker 100...

Page 92: ...92...

Page 93: ...fully insert it Note For better performance adiffuser band covers the light path holes on the adapter Do not remove the band 4 Remove the cap from one HR Monochloramine Diluent vial Use a glass pipet...

Page 94: ...2 Use a Class A volumetric pipet to transfer 2 00 mL of Nitrogen Ammonia Standard Solution 100 mg L as NH3 N into a flask 3 Dilute to volume with organic free water Cap and mix thoroughly This is the...

Page 95: ...this solution within 1 hour of preparation Method Performance Precision In a single laboratory using a standard solution of 3 5 mg L monochloramine as chlorine and two representative lots of reagent a...

Page 96: ...mg L SiO2 Silver 10 mg L Sulfate 2600 mg L Sulfite 50 mg L SO3 2 Tyrosine 1 mg L as N Urea 10 mg L as N Zinc 5 mg L Table 11 Non interfering Substances Continued Substance Maximum Level Tested Table...

Page 97: ...l Safety Data Sheet MSDS for information specific to the reagent used Instrument Setup This procedure will add the current method as a new Hach program to your DR 850 or DR 890 instrument 1 Turn the i...

Page 98: ...41 61 14 49 42 112 15 248 43 0 16 0 44 110 17 0 45 0 18 0 46 0 19 0 47 10 20 67 48 1 21 108 49 44 22 50 50 0 23 0 51 0 24 0 52 0 25 78 53 0 26 72 54 153 27 50 55 0 28 67 56 255 Table 13 Continued CHLO...

Page 99: ...26415 49 Buffer Powder Pillows pH 8 3 25 pkg 898 68 Nitrogen Ammonia Standard Solution 100 mg L as NH3 N 500 mL 24065 49 Chlorine Solution Voluette Ampule 50 75 mg L 10 mL 16 pkg 14268 10 OPTIONAL AP...

Page 100: ...100...

Page 101: ...hod 330 5 for wastewater and Standard Method 4500 C1 G for drinking water 1 Enter the user program number for Chlorine UHR Press PRGM The display will show PRGM Note If the chlorine is typically less...

Page 102: ...e from the total chlorine reagent is carried over to the free chlorine test monochloramine could interfere 5 Press ZERO The cursor will move to the right then the display will show 0 0 mg L Cl2 6 Remo...

Page 103: ...mple 2 Snap the neck of a HR Chlorine Ampule Standard 50 75 mg L Cl2 Using the TenSette Pipet add 0 1 mL 0 2 mL and 0 3 mL of standard respectively to each cylinder and mix thoroughly 3 Analyze each s...

Page 104: ...sample being tested 3 Correct for volume addition Alkalinity Greater than 250 mg L CaCO3 May not develop full color or color may fade instantly 1 Neutralize to pH 6 7 with 1 N Sulfuric Acid 2 Determin...

Page 105: ...ntil the prompt line shows USER 4 Press the ENTER key 5 Enter 8138 followed by ENTER Monochloramine For conventional free chlorine disinfection beyond the breakpoint monochlora mine concentrations are...

Page 106: ...ine Number Enter 1 12 29 0 2 24 30 0 3 73 31 0 4 0 32 0 5 0 33 0 6 0 34 0 7 0 35 0 8 62 36 0 9 55 37 0 10 23 38 0 11 88 39 0 12 64 40 0 13 113 41 0 14 242 42 0 15 18 43 0 16 0 44 110 17 0 45 0 18 0 46...

Page 107: ...ium Arsenite Solution 5 g L 100 mL MDB 1047 32 Sodium Hydroxide Standard Solution 1 00 N 100 mL MDB 1045 32 Sulfuric Acid Standard Solution 1 000 N 100 mL MDB 1270 32 Water deionized 4 L 272 56 OPTION...

Page 108: ...108...

Page 109: ...thod 330 5 for wastewater and Standard Method 4500 C1 G for drinking water 1 Enter the user program number for Chlorine UHR Press PRGM The display will show PRGM Note If the chlorine is typically less...

Page 110: ...ne is present 7 Press TIMER ENTER A 3 minute reaction period will begin 8 Within 3 minutes after the timer beeps place the sample cell into the instrument Cover the sample cell tightly with the instru...

Page 111: ...determinations If trace iodide from the total chlorine reagent is carried over to the free chlorine test monochloramine could interfere A common error in testing for chlorine is failure to obtain a re...

Page 112: ...ne added volume of standard added label value of Cl 2standard ampule sample volume volume of standard added Interfering Substance Interference Levels and Treatments Acidity Greater than 150 mg L CaCO3...

Page 113: ...ey 3 Press the DOWN arrow key until the prompt line shows USER 4 Press the ENTER key 5 Enter 8138 followed by ENTER 6 Key the number in the Enter column corresponding to line number 1 on the display P...

Page 114: ...0 34 0 7 0 35 0 8 62 36 0 9 55 37 0 10 23 38 0 11 88 39 0 12 64 40 0 13 113 41 0 14 242 42 0 15 18 43 0 16 0 44 110 17 0 45 0 18 0 46 0 19 0 47 10 20 67 48 0 21 108 49 180 22 50 50 0 23 0 51 0 24 0 5...

Page 115: ...ium Arsenite Solution 5 g L 100 mL MDB 1047 32 Sodium Hydroxide Standard Solution 1 00 N 100 mL MDB 1045 32 Sulfuric Acid Standard Solution 1 000 N 100 mL MDB 1270 32 Water deionized 4 L 272 56 OPTION...

Page 116: ...116...

Page 117: ...drinking water 1 Enter the stored program number for free and total chlorine Cl2 powder pillows Press PRGM The display will show PRGM Note For most accurate results perform a Reagent Blank Correction...

Page 118: ...into the cell holder Tightly cover the sample cell with the instrument cap Note Perform Step 9 within one minute of reagent addition 9 Press READ The cursor will move to the right then the result in...

Page 119: ...4 Place the blank into the cell holder Tightly cover the sample cell with the instrument cap 5 Press ZERO The cursor will move to the right then the display will show 0 00 mg L Cl2 Note If Reagent Bla...

Page 120: ...ample containers are rinsed thoroughly with deionized or distilled water after use only occasional pretreatment is necessary Do not use the same sample cells for free and total chlorine If trace iodid...

Page 121: ...ple Swirl to mix c Re zero the instrument using the original sample the blank d Place the spiked sample in the cell holder and press READ Record the results e Calculate the concentration of mg L chlor...

Page 122: ...n a single laboratory using a standard solution of 1 00 mg L chlorine and two representative lots of AccuVac Ampuls with the instrument a single operator obtained a standard deviation of 0 01 mg L chl...

Page 123: ...ot then add the same amount to the sample being tested Correct for volume addition See Section 1 Correcting for Volume Additions Bromine Interferes at all levels Chlorine Dioxide Interferes at all lev...

Page 124: ...Arsenite 5 g L 100 mL MDB 1047 32 Sodium Hydroxide Standard Solution 1 000 N 100 mL MDB 1045 32 Sulfuric Acid Standard Solution 1 000 N 100 mL MDB 1270 32 Water deionized 4L 272 56 OPTIONAL APPARATUS...

Page 125: ...for wastewater and Standard Method 4500 Cl G for drinking water 1 Enter the stored program number for total chlorine Cl2 powder pillows Press PRGM The display will show PRGM Note For most accurate re...

Page 126: ...st Dispenser for Total Chlorine can be used in place of the powder pillows in step 7 9 After the timer beeps place the prepared sample into the cell holder Tightly cover the sample cell with the instr...

Page 127: ...ly and cannot be preserved for later analysis 4 Place the blank into the cell holder Tightly cover the sample cell with the instrument cap 5 Press ZERO The cursor will move to the right then the displ...

Page 128: ...at least 1 hour Rinse thoroughly with deionized or distilled water If sample containers are rinsed thoroughly with deionized or distilled water after use only occasional pre treatment is necessary 9...

Page 129: ...is immediately Accuracy Check Standard Additions Method using powder pillows a Snap the top off a LR Chlorine PourRite Ampule Standard Solution b Use a TenSette Pipet to add 0 1 mL of the standard to...

Page 130: ...Method Performance Precision In a single laboratory using a standard solution of 1 00 mg L chlorine and two lots of reagents with the instrument a single operator obtained standard deviations of 0 01...

Page 131: ...Volume Additions Alkalinity Greater than 250 mg L CaCO3 May not develop full color or color may fade instantly Neutralize to pH 6 7 with 1 N sulfuric acid Determine amount to be added on separate sam...

Page 132: ...gent AccuVac Ampuls 1ampul 25 pkg 25030 25 Beaker 50 mL 1 each 500 41H OPTIONAL REAGENTS Description Unit Cat No Chlorine Standard Solution PourRite ampule 25 30 mg L Cl2 20 pkg 26300 20 DPD Total Chl...

Page 133: ...e For most accurate results perform a Reagent Blank Correction using deionized water see Section 1 2 Press 10 ENTER The display will show mg L Cl2 and the ZERO icon 3 Insert the COD TNT Adapter into t...

Page 134: ...Note Fill to the top of the Hach logo oval mark Note A pink color will develop if chlorine is present 10 Cap and invert at least 10 times to dissolve the powder This is the prepared sample Note Use sl...

Page 135: ...common error in testing for chlorine is obtaining an unrepresentative sample If sampling from a tap let the water flow for at least 5 minutes to ensure a representative sample Let the container overfl...

Page 136: ...ting for Volume Additions in the DR 800 Series Procedures Manual Alkalinity Greater than 250 mg L CaCO3 May not develop full color or color may fade instantly Neutralize to pH 6 7 with 1 N sulfuric ac...

Page 137: ...chlorine disinfection beyond the breakpoint typical monochloramine concentrations are very low If monochloramine is present in the sample its interference in the free chlorine test depends on the sam...

Page 138: ...odium Arsenite 5 g L 100 mL MDB 1047 32 Sodium Hydroxide Standard Solution 1 000 N 100 mL MDB 1045 32 Sulfuric Acid Standard Solution 1 000 N 100 mL MDB 1270 32 OPTIONAL APPARATUS Beaker 50 mL each 50...

Page 139: ...139...

Page 140: ...140...

Page 141: ...For most accurate results perform a Reagent Blank Correction using deionized water see Section 1 2 Press 10 ENTER The display will show mg L Cl2 and the ZERO icon 3 Insert the COD TNT Vial Adapter in...

Page 142: ...nk color will develop if chlorine is present 9 Cap and invert at least 10 times to dissolve the powder This is the prepared sample Note Use slow deliberate inversion for complete recovery Ten inversio...

Page 143: ...A common error in testing for chlorine is obtaining an unrepresentative sample If sampling from a tap let the water flow for at least 5 minutes to ensure a representative sample Let the container ove...

Page 144: ...L CaCO3 May not develop full color or color may fade instantly Neutralize to pH 6 7 with 1 N sulfuric acid Determine amount to be added on separate sample aliquot then add the same amount to the samp...

Page 145: ...he reagent to iodine The iodine reacts with DPD N N diethyl p phenylenediamine along with free chlorine present in the sample to form a red color which is proportional to the total chlorine concentrat...

Page 146: ...on 5 g L 100 mL MDB 1047 32 Sodium Hydroxide Standard Solution 1 00 N 100 mL MDB 1045 32 Sulfuric Acid Standard Solution 1 000 N 100 mL MDB 1270 32 OPTIONAL APPARATUS Beaker 50 mL each 500 41H PourRit...

Page 147: ...show PRGM 2 Press 112 ENTER The display will show mg L ClO2 and the ZERO icon 3 Fill a sample cell with 10 mL of sample the blank Note Samples must be analyzed immediately and cannot be preserved for...

Page 148: ...p 9 within one minute of reagent addition 8 Allow 30 seconds for undissolved powder to settle Place the prepared sample into the cell holder Tightly cover the sample cell with the instrument cap Note...

Page 149: ...strument cap Note For best results run a reagent blank using deionized water as the sample Subtract the blank value from the sample reading to obtain the final result See Reagent Blank Correction in S...

Page 150: ...ry A common error in testing for chlorine dioxide is introduced when a representative sample is not obtained If sampling from a tap let the water flow for at least 5 minutes to ensure a representative...

Page 151: ...umetric flask Dilute to the line with chlorine demand free deionized water Invert to mix Method 2 a Dilute 1 drop of commercial 5 chlorine bleach in 1 liter of chlorine demand free deionized water Use...

Page 152: ...amount to be added on separate sample aliquot then add the same amount to the sample being tested Correct for volume addition see Section 1 Correction For Volume Additions in the DR 800 Procedures Man...

Page 153: ...wait one minute 4 Add 3 drops sodium arsenite 5 g L and mix 5 Analyze 10 mL of the treated sample as described in the procedure 6 Subtract the result of this test from the original analysis to obtain...

Page 154: ...s 28023 00 Potassium Iodide Solution 30 g L 100 mL MDB 343 32 Sodium Arsenite 5 g L 100 mL MDB 1047 32 Sodium Hydroxide Standard Solution 1 000 N 100 mL MDB 1045 32 Sulfuric Acid Standard Solution 1 0...

Page 155: ...water see Section 1 2 Press 23 ENTER The display will show mg L CN and the ZERO icon Note Adjust the pH of stored samples before analysis 3 Fill a sample cell with 10 mL of sample Note Samples at less...

Page 156: ...CyaniVer 5 Cyanide Reagent Powder for more than 30 seconds after the addition of the CyaniVer 4 Cyanide Reagent Powder will give lower test results Note Accuracy is not affected by undissolved CyaniVe...

Page 157: ...sodium hydroxide if necessary Store the samples at 4 C 39 F or less Samples preserved in this manner can be stored for 14 days Before testing samples preserved with 5 0 N sodium hydroxide or samples t...

Page 158: ...irl to mix The solution will turn blue if oxidizing agents are present d If Step c suggests the presence of oxidizing agents add two level 1 g measuring spoonfuls of ascorbic acid per liter of sample...

Page 159: ...ples with sodium hydroxide until the following pretreatment is performed The effect of fatty acids can be minimized as follows a Acidify 500 mL of sample to pH 6 or 7 with Acetic Acid Solution Prepare...

Page 160: ...le is highly turbid it should first be filtered before use in Steps 3 and 12 Filter using the labware listed under Optional Apparatus The test results should then be recorded as soluble cyanide Oxidiz...

Page 161: ...Solution to the sample Swirl to mix The sample should be colorless c Add Bromine Water drop wise until a blue color appears Count the number of drops and swirl the sample after the addition of each d...

Page 162: ...n be determined The sample is not distilled and the final reading is multiplied by 2 2 The result is mg L thiocyanate The distillate can be tested and treated for sulfide after the last step of the di...

Page 163: ...3 Cyanide Reagent Powder Pillows 1 pillow 100 pkg 21068 69 CyaniVer 4 Cyanide Reagent Powder Pillows 1 pillow 100 pkg 21069 69 CyaniVer 5 Cyanide Reagent Powder Pillows 1 pillow 100 pkg 21070 69 REQU...

Page 164: ...nd Support Apparatus 230 Vac 50 Hz each 22744 02 Dropper plastic each 6080 00 Filter Paper folded 12 5 cm 100 pkg 1894 57 Flask volumetric Class A 1000 mL each 14574 53 Flask volumetric Class A 250 mL...

Page 165: ...g is required for highly turbid samples 4 Place the blank into the cell holder Tightly cover the sample cell with the instrument cap 5 Press ZERO The cursor will move to the right then the display wil...

Page 166: ...aily c Testing the 20 mg L solution should give test results of about 20 mg L cyanuric acid Method Performance Precision In a single laboratory using a standard solution of 25 0 mg L cyanuric acid and...

Page 167: ...precipitation reaction low levels of cyanuric acid less than 7 mg L are not detected by this method REQUIRED REAGENTS AND APPARATUS Quantity Required Description Per Test Unit Cat No Cyanuric Acid 2 R...

Page 168: ...168...

Page 169: ...ZERO icon 3 Pipet 10 0 mL of sample into a dry 10 mL sample cell the prepared sample 4 Measure 10 0 mL of deionized water into a second dry sample cell the blank Note The sample and blank should be at...

Page 170: ...g AccuVac Ampuls 1 Enter the stored program number for fluoride F AccuVac Ampuls Press PRGM The display will show PRGM 2 Press 28 ENTER The display will show mg L F and the ZERO icon 3 Collect at leas...

Page 171: ...cover the ampule with the instrument cap 8 Press ZERO The cursor will move to the right then the display will show 0 0 mg L F 9 Place the AccuVac Ampul containing the sample into the instrument Tight...

Page 172: ...w keys to scroll to the STD setup option Press ENTER to activate the option Then enter 1 80 to edit the standard concentration to match that of the standard used Press ENTER to complete the adjustment...

Page 173: ...to 3 0 mg L aluminum Most interferences can be eliminated by distilling the sample from an acid solution as described below a Set up the distillation apparatus for the general purpose distillation Se...

Page 174: ...ratus listing Pollution Prevention and Waste Management SPADNS Reagent contains sodium arsenite Final solutions will contain sodium arsenite D004 in sufficient concentration to be regulated as hazardo...

Page 175: ...ate ACS 113 g 334 14 Sodium Arsenite Solution 100 mL MDB 1047 32 StillVer Distillation Solution 500 mL 446 49 OPTIONAL APPARATUS AccuVac Snapper Kit each 24052 00 Cylinder graduated 100 mL each 508 42...

Page 176: ...176...

Page 177: ...ress 27 ENTER The display will show mg L F and the ZERO icon 3 Pipet 10 0 mL of sample into a dry 10 mL sample cell the prepared sample 4 Measure 10 0 mL of deionized water into a second dry sample ce...

Page 178: ...AccuVac Ampuls 1 Enter the stored program number for fluoride F AccuVac Ampuls Press PRGM The display will show PRGM 2 Press 28 ENTER The display will show mg L F and the ZERO icon 3 Collect at least...

Page 179: ...t cap 8 Press ZERO The cursor will move to the right then the display will show 0 0 mg L F 9 Place the AccuVac Ampul containing the sample into the instrument Tightly cover the sample cell with the in...

Page 180: ...keys to scroll to the STD setup option Press ENTER to activate the option Then enter 1 80 to edit the standard concentration to match that of the standard used Press ENTER to complete the adjustment S...

Page 181: ...ours before making the final reading will eliminate the effect of up to 3 0 mg L aluminum Most interferences can be eliminated by distilling the sample from an acid solution as described below a Set u...

Page 182: ...tewater samples require distillation See Optional Apparatus for Distillation Apparatus listing Pollution Prevention and Waste Management SPADNS 2 Reagent contains a non toxic proprietary reducing agen...

Page 183: ...mL 405 20 Silver Sulfate ACS 113 g 334 14 StillVer Distillation Solution 500 mL 446 49 OPTIONAL APPARATUS AccuVac Snapper Kit each 24052 00 Cylinder graduated 100 mL each 508 42 Cylinder graduated 25...

Page 184: ...184...

Page 185: ...ture should be 21 29 C 70 84 F 4 Add 1 0 mL of Calcium and Magnesium Indicator Solution using a 1 0 mL measuring dropper Stopper Invert several times to mix 5 Add 1 0 mL of Alkali Solution for Calcium...

Page 186: ...ell holder Tightly cover the sample cell with the instrument cap 12 Press READ The cursor will move to the right then the result in mg L magnesium hardness as CaCO3 will be displayed 13 Without removi...

Page 187: ...ated Detection Limit The estimated detection limit for program 30 is 0 13 mg L magnesium hardness and 0 08 mg L calcium hardness For more information on the estimated detection limit see Section 1 Int...

Page 188: ...tion gives results as the calcium and magnesium hardness concentrations REQUIRED REAGENTS Cat No Hardness Reagent Set 100 Tests 23199 00 Includes 1 22417 32 1 22418 32 1 22419 26 1 22297 26 Quantity R...

Page 189: ...determined 2 Press 33 ENTER The display will show mg L Fe and the ZERO icon 3 Fill a sample cell with 25 mL of sample the blank 4 Place the blank into the cell holder Tightly cover the sample cell wit...

Page 190: ...ter the stored program number for ferrous iron Fe2 AccuVac ampuls Press PRGM The display will show PRGM Note Analyze samples as soon as possible to prevent air oxidation of ferrous iron to ferric whic...

Page 191: ...Undissolved powder does not affect accuracy 8 Press TIMER ENTER A three minute reaction period will begin Note An orange color will form if ferrous iron is present 9 Place the AccuVac ampul into the c...

Page 192: ...single laboratory using an iron standard solution of 2 00 mg L Fe2 and two representative lots of powder pillow reagents with the instrument a single operator obtained a standard deviation of 0 017 mg...

Page 193: ...4 Water deionized 4 L 272 56 OPTIONAL APPARATUS AccuVac Snapper Kit each 24052 00 Balance analytical 115 V 0 1 mg each 28014 01 Balance analytical 230 V 0 1 mg each 28014 02 Clippers for opening powde...

Page 194: ...194...

Page 195: ...mples treat the blank with one 0 1 gram scoop of RoVer Rust Remover Swirl to mix 4 Place the blank into the cell holder Tightly cover the sample cell with the instrument cap 5 Press ZERO The cursor wi...

Page 196: ...ls Press PRGM The display will show PRGM Note Adjust pH of stored samples before analysis Note Determination of total iron requires a digestion prior to analysis see Section 2 2 Press 33 ENTER The dis...

Page 197: ...if iron is present Note Accuracy is not affected by undissolved powder 8 Press TIMER ENTER A three minute reaction period will begin Note Samples containing visible rust should be allowed to react at...

Page 198: ...0 3 mL of standard respectively to three 25 mL samples and mix thoroughly c For analysis using AccuVac Ampuls transfer solutions to dry clean 50 mL beakers to facilitate filling of the ampuls For ana...

Page 199: ...uggested Treatments Interfering Substance Interference Level and Treatment Calcium Ca2 No effect at less than 10 000 mg L as CaCO3 Chloride Cl No effect at less than 185 000 mg L Copper Cu2 No effect...

Page 200: ...L 28337 49 Drinking Water Standard Metals HR Cu Fe Mn 500 mL 28336 49 Hydrochloric Acid Standard Solution 6 N 500 mL 884 49 Hydrochloric Acid ACS 500 mL 134 49 Iron Standard Solution 100 mg L 100 mL 1...

Page 201: ...Flask volumetric Class A 100 mL each 14574 42 Hot Plate 4 diameter 120 VAC each 12067 01 Hot Plate 4 diameter 240 VAC each 12067 02 pH Meter sension 1 portable with electrode each 51700 10 pH Indicat...

Page 202: ...202...

Page 203: ...inse glassware with 1 1 Hydrochloric Acid Solution Rinse again with deionized water This removes iron deposits which can cause slightly high results 4 Add the contents of one FerroMo Iron Reagent 1 Po...

Page 204: ...25 mg L Fe b Use the TenSette Pipet to add 0 2 0 4 and 0 6 mL of standard to three 50 mL samples Swirl gently to mix c Analyze each sample as described above The iron concentration should increase by...

Page 205: ...m 38 is 0 03 mg L Fe For more information on the estimated detection limit see Section 1 Interferences A sample pH of less than 3 or greater than 4 after reagent addition may inhibit color formation c...

Page 206: ...00 mg L Fe 100 mL 14175 42 Iron Standard Solution PourRite Ampule 25 mg L Fe 2 mL 20 pkg 24629 20 Sodium Hydroxide Standard Solution 1 0 N 100 mL MDB 1045 32 Sodium Hydroxide Standard Solution 5 0 N 1...

Page 207: ...te Adjust the pH of stored samples before analysis 2 Press 39 ENTER The display will show mg L Fe and the ZERO icon Note Total iron determination needs a prior digestion Use any of the procedures in D...

Page 208: ...ment while the timer is running Press ZERO The cursor will move to the right then the display will show 0 00 mg L Fe If Reagent Blank Correction is on the display may flash limit See Section 1 8 After...

Page 209: ...see Interferences Note Rinse glassware with a 1 1 hydrochloric acid and deionized water before use to avoid errors due to iron deposits on the glass 4 Fill a TPTZ Iron AccuVac Ampul with sample Note K...

Page 210: ...for volume additions see Correction for Volume Additions in Section 1 Accuracy Check Standard Additions Method Powder Pillows a Snap the neck off a PourRite Iron Ampule Standard 25 mg L Fe b Use the...

Page 211: ...concentration should increase by 0 1 mg L for each 0 1 mL addition of standard f If these increases do not occur see Standard Additions in Section 1 for more information Standard Solution Method Prep...

Page 212: ...1 2 mg L Cobalt Greater than 0 05 mg L Color or turbidity If the sample is turbid add one 0 1 g scoop of RoVer Rust Remover to the blank in Step 6 Step 3 for AccuVac procedure Swirl to mix Copper Gre...

Page 213: ...2540 49 RoVer Rust Remover 454 g 300 01 Sodium Hydroxide Standard Solution 1 0 N 100 mL MDB 1045 32 Sodium Hydroxide Standard Solution 5 0 N 100 mL MDB 2450 32 Sulfuric Acid Standard Solution 100 mL...

Page 214: ...214...

Page 215: ...anganese determination perform a digestion see Section 2 Note Adjust the pH of stored samples before analysis 4 Place the blank into the cell holder Tightly cover the sample cell with the instrument c...

Page 216: ...ion Accuracy Check Standard Additions Method a Snap the neck off a Manganese Voluette Ampule Standard Solution 250 mg L Mn b Use the TenSette Pipet to add 0 1 0 2 and 0 3 mL of standard respectively t...

Page 217: ...representative lots of reagent with the instrument a single operator obtained a standard deviation of 0 18 mg L Mn Estimated Detection Limit The estimated detection limit for program 41 is 0 2 mg L Mn...

Page 218: ...32 Water deionized 4 L 272 56 OPTIONAL APPARATUS Ampule Breaker Kit each 21968 00 Flask Erlenmeyer 250 mL each 505 46 Flask volumetric Class A 50 mL each 14574 41 Flask volumetric Class A 100 mL each...

Page 219: ...a 25 mL mixing graduated cylinder with 20 mL of the sample Note Filter turbid samples using the labware listed under Optional Apparatus 4 Add the contents of one Molybdenum 1 Reagent Powder Pillow to...

Page 220: ...itions in Section 1 for more information Standard Solution Method Prepare a 2 0 mg L molybdenum standard solution by pipetting 10 mL of a 10 mg L Molybdenum Standard Solution into a 50 9 Insert the bl...

Page 221: ...Section 1 Interferences Interference studies were conducted by preparing a molybdenum standard solution 2 mg L Mo6 as well as a solution of the potential interfering ion When the standard solution con...

Page 222: ...rops of an acid or base such as 1 0 N Sulfuric Acid Standard Solution or 1 0 N Sodium Hydroxide Standard Solution If a significant volume of acid or base is used correct the result by dividing the tot...

Page 223: ...r and sensitizing agent to give a stable blue complex REQUIRED REAGENTS Molybdenum Reagent Set 20 mL sample 100 tests 24494 00 Includes 1 23524 49 1 23525 12 Quantity Required Description Per Test Uni...

Page 224: ...rolls pkg 391 33 Pipet TenSette 0 1 to 1 0 mL each 19700 01 Pipet Tips for 19700 01 TenSette Pipet 50 pkg 21856 96 Pipet volumetric 10 00 mL Class A each 14515 38 Pipet Filler safety bulb each 14651...

Page 225: ...two cells with 10 mL of sample Label one cell Free Ammonia and one cell Monochloramine 4 Place the Monochloramine cell into the instrument so that the cell tab is at the two o clock position Make sur...

Page 226: ...ake sure the sample cell tab is completely seated in the cell holder slot Tightly cover the sample cell with the instrument cap 13 Press READ The cursor will move to the right then the result in mg L...

Page 227: ...Press TIMER ENTER A five minute reaction period will begin Note The color development time depends on the sample temperature See Table 1 20 After the timer has expired press EXIT 21 Place the Free Am...

Page 228: ...intended for finished chloraminated drinking water samples that have a measurable combined total chlorine disinfectant residual Samples where the disinfectant residual has disappeared and samples whi...

Page 229: ...cap Continue with the analysis at step 2 using the pretreated sample as the Free Ammonia cell Accuracy Check Monochloramine Program 110 1 Prepare the following monochloramine standard fresh before us...

Page 230: ...d it cannot be used for accuracy verification of the Free Ammonia test 10 Quantitatively transfer the monochloramine solution to a clean 100 mL Class A volumetric flask Dilute to the mark with organic...

Page 231: ...following all steps of the Monochloramine and Free Ammonia procedure Method Performance Monochloramine Test Precision In a single laboratory using a monochloramine standard solution of 2 10 mg L Cl2...

Page 232: ...roughout the procedure Consult the Material Safety Data Sheet MSDS for information specific to the reagent used REQUIRED REAGENTS Quantity Required Description Per Test Unit Cat No Free Ammonia Reagen...

Page 233: ...14651 00 Pipet TenSette 0 1 to 1 0 mL each 19700 01 Pipet Tips for 19700 01 TenSette Pipet 50 pkg 21856 96 Pipet Mohr Glass 10 mL each 20934 38 Pipet Volumetric Class A 2 0 mL each 14515 36 Pipet Vol...

Page 234: ...234...

Page 235: ...Note For most accurate results perform a Reagent Blank Correction using deionized water see Section 1 2 Press 51 ENTER The display will show mg L NO3 N and the ZERO icon Note For alternate forms NO3...

Page 236: ...f sample the blank Wipe off any fingerprints or liquid 8 Place the blank into the cell holder Tightly cover the sample cell with the instrument cap 9 When the timer beeps press ZERO The cursor will mo...

Page 237: ...begin Invert the ampul repeatedly back and forth until the timer beeps Wipe off any liquid or fingerprints Note Mixing time and technique influence color development For most accurate results do succ...

Page 238: ...0 N Sodium Hydroxide Standard Solution Do not use mercury compounds as preservatives Correct the test result for volume additions see Correction for Volume Additions Section 1 for more information 9 P...

Page 239: ...NO3 N listed under Optional Reagents as the sample and perform the procedure as described above Standard Adjust To adjust the calibration curve using the reading obtained with the 10 0 mg L standard...

Page 240: ...the drain See Section 3 for more information on proper disposal of these materials Interfering Substance Interference Levels and Treatments Chloride Chloride concentrations above 100 mg L will cause...

Page 241: ...l Solution 29 mL 2112 20 Sodium Hydroxide Standard Solution 5 0 N 50 mL 2450 26 Sulfuric Acid ACS 500 mL 979 49 Water deionized 4 L 272 56 OPTIONAL APPARATUS AccuVac Snapper Kit each 24052 00 Cylinder...

Page 242: ...242...

Page 243: ...tion using deionized water see Section 1 2 Press 55 ENTER The display will show mg L NO3 N and the ZERO icon Note For alternate forms NO3 press the CONC key 3 Fill a 25 mL graduated mixing cylinder to...

Page 244: ...r any cadmium particles 8 Add the contents of one NitriVer 3 Nitrite Reagent Powder Pillow to the sample cell the prepared sample Cap the cell and shake gently for 30 seconds Note A pink color will fo...

Page 245: ...utralize with 5 0 N Sodium Hydroxide Standard Solution Do not use mercury compounds as preservatives Correct the test result for volume additions see Correction for Volume Additions Section 1 for more...

Page 246: ...water Use this standard in place of sample in Step 3 Standard Adjust To adjust the calibration curve using the reading obtained with the 0 20 mg L standard solution press the SETUP key and scroll usin...

Page 247: ...ride concentrations above 100 mg L will cause low results The test may be used at high chloride concentrations seawater but a calibration must be done using standards spiked to the same chloride conce...

Page 248: ...Solution 5 0 N 50 mL SCDB 2450 26 Sulfuric Acid ACS 500 mL 979 49 Water deionized 4 L 272 56 OPTIONAL APPARATUS Ampule Breaker each 21968 00 Dropper for 29 mL bottle each 2258 00 Flask volumetric Clas...

Page 249: ...en NO2 N powder pillows Press PRGM The display will show PRGM Note For most accurate results perform a Reagent Blank Correction using deionized water see Section 1 2 Press 60 ENTER The display will sh...

Page 250: ...ment cap Note Wiping with a damp cloth followed by a dry pne removes fingerprints and other marks 8 Press ZERO The cursor will move to the right then the display will show 0 000 mg L NO2 N Note If Rea...

Page 251: ...Keep the tip immersed while the ampul fills completely 4 Quickly invert the ampul several times to mix Wipe off any liquid or fingerprints Note Accuracy is not affected by undissolved powder 5 Press T...

Page 252: ...standard to 500 mL in a volumetric flask Prepare this solution immediately before use Run the test using the 0 100 mg L NO2 N standard in place of the sample Results should be between 0 090 and 0 110...

Page 253: ...e by causing precipitation Bismuth ions Interfere by causing precipitation Chloroplatinate ions Interfere by causing precipitation Cupric ions Cause low results Ferric ions Interfere by causing precip...

Page 254: ...US Description Unit Cat No AccuVac Snapper Kit each 24052 00 Flask volumetric 250 mL each 14574 46 Flask volumetric 500 mL each 14574 49 Pipet serological 10 mL each 532 38 Pipet TenSette 1 to 10 mL e...

Page 255: ...insert Note For increased performance a diffuser band covers the light path holes on the adapter Do not remove the diffuser band 4 Fill a Test N Tube NitriVer 3 Nitrite vial with 5 mL of sample Cap an...

Page 256: ...ely before use Run the test using the 0 100 mg L NO2 N standard in place of the sample Results should be between 0 090 and 0 110 mg L NO2 N 9 Cover the sample cell tightly with the instrument cap 10 P...

Page 257: ...Interfering Substance Interference Levels Antiminous ions Interfere by causing precipitation Auric ions Interfere by causing precipitation Bismuth ions Interfere by causing precipitation Chloroplatin...

Page 258: ...be Rack 1 3 each 18641 00 Pipet TenSette 1 to 10 mL 1 each 19700 10 Pipet Tips for 19700 10 TenSette Pipet 1 50 pkg 21997 96 OPTIONAL REAGENTS Nitrite Standard Solution 250 mg L as NO2 N 500mL 23402 4...

Page 259: ...Fill a second sample cell with 10 mL of the sample 5 Add the contents of one Ammonia Salicylate Reagent Powder Pillow to each sample cell Cap both cells and shake to dissolve 6 Press TIMER ENTER A thr...

Page 260: ...t before testing the stored sample warm to room temperature and neutralize with 5 0 N Sodium Hydroxide Standard Solution Correct the test result for volume additions see Correction for Volume Addition...

Page 261: ...nitrogen standard by diluting 4 00 mL of the Ammonia Nitrogen Standard Solution 10 mg L to 100 mL with deionized water Or using the TenSette Pipet prepare a 0 40 mg L ammonia nitrogen standard by dil...

Page 262: ...ration as the original sample Run the procedure on this solution to determine the interference due to iron Subtract this value from the result in Step 12 obtained on the original sample Magnesium Grea...

Page 263: ...L 979 49 Sulfuric Acid Standard Solution 1 0 N 100 mL MDB 1270 32 Water deionized 4 L 272 56 OPTIONAL APPARATUS Cylinder graduated polypropylene 500 mL each 1081 49 Distillation Heater and Support App...

Page 264: ...264...

Page 265: ...reased performance a diffuser band covers the light path holes on the adapter Do not remove the diffuser band 4 Remove the caps from 2 AmVer Diluent Reagent vials Add 2 mL of sample to one vial the sa...

Page 266: ...Sette Pipet to add 0 1 0 2 and 0 3 mL of standard to three 25 mL samples Mix thoroughly 9 Wipe the outside of the vials with a towel After the timer beeps place the blank into the adapter Tightly cove...

Page 267: ...ard deviation of 0 02 mg L NH3 N Estimated Detection Limit The estimated detection limit for program 66 is 0 08 mg L NH3 N For more information on the estimated detection limit see Section 1 Interfere...

Page 268: ...w Range TNT 25 tests 26045 45 Includes 1 23952 66 1 23954 66 1 272 42 50 AmVer Low Range Vials Quantity Required Description Per Test Unit Cat No AmVer Diluent Reagent Low Range Test N Tube 2 vials 50...

Page 269: ...ffluent Standard Inorganics NH3 N NO3 N PO4 COD SO4 TOC 500 mL 28332 49 Water deionized 4 L 272 56 OPTIONAL APPARATUS Ampule Breaker Kit each 21968 00 Cylinder graduated mixing 25 mL Class A each 508...

Page 270: ...270...

Page 271: ...t drops into place Then push down to fully insert it Note For increased performance a diffuser band covers the light path holes on the adapter Do not remove the diffuser band 4 Remove the caps from 2...

Page 272: ...y will show 0 mg L NH3 N 11 Place the prepared sample in the adapter Push straight down on the top of the vial until it seats solidly into the adapter Note Do not move the vial from side to side as th...

Page 273: ...and 0 6 mL of standard to three 25 mL samples Swirl to mix c Analyze each sample as described above The ammonia concentration should increase approximately 1 2 mg L NH3 N for each 0 2 mL of standard...

Page 274: ...300 000 mg L as CaCO3 Iron Eliminate iron interference as follows 1 Determine the amount of iron present in the sample using one of the total iron procedures 2 Add the same iron concentration to the...

Page 275: ...stes by the Federal RCRA Collect cyanide solutions for disposal as reactive D001 waste Be sure cyanide solutions are stored in a caustic solution with pH 11 to prevent release of hydrogen cyanide gas...

Page 276: ...49 Water deionized 4 L 272 56 OPTIONAL APPARATUS Cylinder 25 mL graduated mixing each 20886 40 Distillation Apparatus Set general purpose each 22653 00 Heater and Support Apparatus for distillation 1...

Page 277: ...Vials 5 Pipet 1 mL of sample into 1 TIN Diluent Vial the sample Pipet 1 mL of deionized water into the other vial the blank Cap the vials and shake for 30 seconds to mix 6 Snap the necks off two Tota...

Page 278: ...oughly to dissolve the powder Note A green color will develop if inorganic nitrogen is present 13 The display will show 15 00 TIMER 2 Press ENTER A 15 minute reaction period will begin 14 After the ti...

Page 279: ...Check Standard Additions Method a Fill three 25 mL graduated mixing cylinders with 25 mL of sample b Snap the neck off a fresh High Range Nitrate Nitrogen PourRite Ampule Standard 500 mg L NO3 N c Us...

Page 280: ...n load in water or wastewater samples This test is most applicable for monitoring an industrial process stream or a wastewater treatment stream where it is important to track the inorganic nitrogen lo...

Page 281: ...ions reduce nitrate and nitrite to ammonia in a basic environment After centrifugation to remove solids the ammonia is combined with chlorine to form monochloramine Monochloramine reacts with salicyl...

Page 282: ...urate Reagent Powder Pillows for 5 mL sample 2 pillows 50 pkg 23954 66 REQUIRED APPARATUS Centrifuge 115V 1 each 26765 00 Centrifuge 230V 1 each 26765 02 COD TNT Vial Adapter 1 each 48464 00 Funnel mi...

Page 283: ...cator Paper 1 to 11 pH 5 rolls pkg 391 33 Pipet volumetric Class A 2 0 mL each 14515 36 Pipet Tips for 19700 01 TenSette Pipet 1000 pkg 21856 28 PourRite Ampule Breaker each 24846 00 For Technical Ass...

Page 284: ...284...

Page 285: ...he sample while pipetting if suspended solids are present 4 If chloride is not present in significant amounts pipet 0 50 mL of homogenized sample into a Mn III COD vial Cap and invert several times to...

Page 286: ...te Samples can be digested up to 4 hours to oxidize more resistant organics The prepared blank must be treated in the same manner Note See DRB 200 user manual for selecting pre programmed temperature...

Page 287: ...ill show 0 mg L COD 12 If the chloride removal was done make sure the filter disc is not suspended in the middle of the vial it can interfere with the instrument reading Move it with gentle swirling o...

Page 288: ...00 26 mg L COD An 800 mg L COD solution can also be purchased directly from Hach see Optional Reagents Method Performance for Manganic III COD without the chloride removal procedure Precision In a sin...

Page 289: ...ess when it reacts with organic matter It typically oxidizes about 80 of the organic compounds Studies have shown that the reactions are highly reproducible and test results correlate closely to Bioch...

Page 290: ...1 0 mL 1 each 19700 01 Pipet Tips for 19700 01 TenSette 2 1000 pkg 21856 28 Test Tube Rack stainless steel 1 each 18641 00 OPTIONAL REAGENTS COD Standard Solution 800 mg L COD 200 mL 26726 29 Oxygen...

Page 291: ...the flask on a stir plate and stir at a moderate speed for 10 minutes 5 Label two Low Range Acid Digestion vials sample and reagent blank Note A reagent blank is required for each series of samples 6...

Page 292: ...rack Allow the vials to cool for one hour for accurate results 12 Insert the COD TNT Adapter into the cell holder by rotating the adapter until it drops into place Then push down to fully insert it No...

Page 293: ...ive samples 17 Tightly cover the vial assembly with the instrument cap 18 Press ZERO The cursor will move to the right then the display will show 0 0 mg L C 19 Wipe the sample vial assembly with a dam...

Page 294: ...ass A volumetric flask Dilute to volume using Organic Free Reagent Water Stopper and mix thoroughly Prepare this standard fresh daily Standard Additions Method a Prepare a 150 mg L C standard by trans...

Page 295: ...L C Interferences The following have been tested for interference and found not to interfere up to the indicated levels Table 1 Non interfering Substances Substance Maximum Level Tested Aluminum 10 mg...

Page 296: ...nner ampule The adsorption of carbon dioxide into the indicator forms carbonic acid Carbonic acid changes the pH of the indicator solution which in turn changes the color The amount of color change is...

Page 297: ...7 96 Stir Bar Magnetic 1 each 45315 00 Wipes Disposable Kimwipes 1 280 pkg 20970 00 OPTIONAL REAGENTS Potassium Acid Phthalate 500 g 315 34 Sulfuric Acid Reagent Solution 5 25 N 100 mL MDB 2449 32 TOC...

Page 298: ...298...

Page 299: ...stir plate and stir at a moderate speed for 10 minutes 5 Label two Mid Range Acid Digestion vials sample and reagent blank Note A reagent blank is required for each series of samples 6 Using a funnel...

Page 300: ...rack Allow the vials to cool for one hour for accurate results 12 Insert the COD TNT Adapter into the cell holder by rotating the adapter until it drops into place Then push down to fully insert it No...

Page 301: ...e the sample vial assembly with a damp towel followed by a dry one to remove fingerprints or other marks 20 Place the sample vial assembly in the adapter Push straight down on the top of the vial asse...

Page 302: ...Alternatively open one ampule of TOC Standard Solution Cat No 27915 05 b Prepare a 100 mg L C standard by transferring 5 00 mL of the stock standard to a 50 mL Class A volumetric flask Dilute to volum...

Page 303: ...nd found not to interfere up to the indicated levels mg L C 95 Confidence Limits 15 5 mg L C 50 6 mg L 75 7 mg L 115 4 mg L 150 6 mg L Table 1 Non interfering Substances Substance Maximum Level Tested...

Page 304: ...on In the outside vial organic carbon in the sample is digested by persulfate and acid to form carbon dioxide During digestion the carbon dioxide diffuses into a pH indicator reagent in the inner ampu...

Page 305: ...17 0 45 128 18 0 46 0 19 0 47 10 20 67 48 0 21 0 49 0 22 0 50 0 23 0 51 0 24 0 52 0 25 0 53 0 26 0 54 25 27 0 55 0 28 0 56 255 1 Turn the instrument on by pressing the ON key 2 Press the SETUP key 3...

Page 306: ...41 00 Pipet TenSette 0 1 to 1 0 mL 1 each 19700 01 Pipet Tips for 19700 01 TenSette Pipet 2 50 pkg 21856 96 Stir Bar Magnetic 1 each 45315 00 Wipes Disposable Kimwipes 1 280 pkg 20970 00 OPTIONAL REAG...

Page 307: ...e flask on a stir plate and stir at a moderate speed for 10 minutes 5 Label two High Range Acid Digestion vials sample and reagent blank Note A reagent blank is required for each series of samples 6 U...

Page 308: ...rack Allow the vials to cool for one hour for accurate results 12 Insert the COD TNT Adapter into the cell holder by rotating the adapter until it drops into place Then push down to fully insert it No...

Page 309: ...ative samples 17 Tightly cover the vial assembly with the instrument cap 18 Press ZERO The cursor will move to the right then the display will show 0 mg L C 19 Wipe the sample vial assembly with a dam...

Page 310: ...ass A volumetric flask Dilute to volume using Organic Free Reagent Water Stopper and mix thoroughly Prepare this standard fresh weekly Standard Additions Method a Prepare a 300 mg L C standard by tran...

Page 311: ...Interferences The following have been tested for interference and found not to interfere up to the indicated levels Table 1 Non interfering Substances Substance Maximum Level Tested Aluminum 10 mg L...

Page 312: ...or reagent in the inner ampule The adsorption of carbon dioxide into the indicator forms carbonic acid Carbonic acid changes the pH of the indicator solution which in turn changes the color The amount...

Page 313: ...1 280 pkg 20970 00 OPTIONAL REAGENTS Oxygen Demand Standard BOD COD TOC 10 mL Ampules 16 pkg 28335 10 Potassium Acid Phthalate 500 g 315 34 Sulfuric Acid Reagent Solution 5 25 N 100 mL MDB 2449 32 TOC...

Page 314: ...314...

Page 315: ...of solids and improves accuracy and reproducibility Note Continue mixing the sample while pipetting if suspended solids are present Chloride Removal Procedure 4 Using a TenSette Pipet or a pipet and...

Page 316: ...7 Prepare a blank see note by repeating Steps 4 6 substituting 9 0 mL of deionized water for the sample Note The reagent blank is stable and can be reused Verify reagent blank quality by measuring th...

Page 317: ...pet 0 60 mL of acidified blank into another CRC Note If the sample does not flow through the CRC increase the vacuum until flow starts then reduce the vacuum to 20 inches of water Proceed as usual All...

Page 318: ...Place each filter in the corresponding Mn III COD Vial use the numbers on the VPD as a guide Note If the sample does not contain suspended solids it is not necessary to transfer the filter to the dig...

Page 319: ...l Then cool the vials to room temperature in a cool water bath or running tap water This usually takes about three minutes Note Occasionally a vial will develop a colorless upper layer and a purple lo...

Page 320: ...vial it can interfere with the instrument reading Move it with gentle swirling or by lightly tapping the vial on the table top 24 Place the sample in the adapter Push straight down on the top of the v...

Page 321: ...00 26 mg L COD An 800 mg L COD solution can also be purchased directly from Hach see Optional Reagents Method Performance for Manganic III COD without the chloride removal procedure Precision In a sin...

Page 322: ...ess when it reacts with organic matter It typically oxidizes about 80 of the organic compounds Studies have shown that the reactions are highly reproducible and test results correlate closely to Bioch...

Page 323: ...ps for 19700 01 TenSette 2 1000 pkg 21856 28 Test Tube Rack stainless steel 1 each 18641 00 Vacuum Pretreatment Device VPD 1 each 49000 00 Vacuum Pump 115 V 1 each 14697 00 Vacuum Pump 230V 1 each 146...

Page 324: ...324...

Page 325: ...ith sample Note Keep the tip immersed while the ampul fills completely 5 Without inverting the ampul immediately place the ampul cap that has been filled with sample securely over the tip of the ampul...

Page 326: ...microbial action mixing travel time and other factors A single dissolved oxygen test rarely reflects the accurate over all condition of a body of water Several samples taken at different times locatio...

Page 327: ...ent vacuum sealed in a 12 mL ampul When the AccuVac ampul is broken open in a sample containing dissolved oxygen a yellow color forms which turns purple as the oxygen reacts with the reagent The color...

Page 328: ...Vac Snapper Kit each 24052 00 AccuVac Drainer each 41036 00 BOD bottle and stopper 300 mL each 621 00 Dissolved Oxygen Meter Portable HQ 10 each 51815 01 Dissolved Oxygen Reagent Set Buret Method 100...

Page 329: ...ment cap 5 Press ZERO The cursor will move to the right then the display will show 0 g L O2 Note If Reagent Blank Correction is on the display may flash limit See Section 1 6 Collect at least 40 mL of...

Page 330: ...checked by following these steps a Fill a 50 mL beaker with sample and add approximately 50 mg sodium hydrosulfite b Immerse the tip of a Low Range Dissolved Oxygen AccuVac Ampul in the sample and br...

Page 331: ...Test Unit Cat No Low Range Dissolved Oxygen AccuVac Ampuls 1 ampul 25 pkg 25010 25 Beaker 50 mL 1 each 500 41H Sample Cell 10 20 25 mL w cap 1 6 pkg 24019 06 OPTIONAL REAGENTS AND APPARATUS AccuVac S...

Page 332: ...332...

Page 333: ...teps for proper collection 4 Collect at least 40 mL of ozone free water blank in another 50 mL beaker Note Ozone free water used for the blank may be deionized water or tap water 5 Fill one Indigo Ozo...

Page 334: ...ultiple measurements during the same day Method Performance Precision In a single laboratory using standard solutions of 0 15 0 28 and 0 96 mg L ozone for the low mid and high range respectively and t...

Page 335: ...ine interference No transfer of sample is needed in the procedure Therefore ozone loss due to sampling is eliminated REQUIRED REAGENTS Quantity Required Description Per Test Unit Cat No Ozone AccuVac...

Page 336: ...336...

Page 337: ...blank 4 Place the blank in the cell holder Tightly cover the sample cell with the instrument cap 5 Press ZERO The cursor will move to the right then the display will show 6 0 PH 6 Fill another cell wi...

Page 338: ...dard solution of pH 7 0 and two lots of reagent with the instrument a single operator obtained a standard deviation of less than 0 1 pH units Estimated Detection Limit The estimated detection limit fo...

Page 339: ...not be analyzed using this method Summary of Method This method uses a sulfonphthalein indicator Phenol Red to determine pH colorimetrically Phenol Red has a working range of pH 6 8 yellow to 8 2 red...

Page 340: ...340...

Page 341: ...uated mixing cylinder Dilute the sample to 50 mL with deionized water Mix well Note Clean glassware with 1 1 hydrochloric acid followed by a deionized water rinse Do not use commercial detergents cont...

Page 342: ...ates to wash glassware Note A specially designed cord adapter is available for performing two digestions with a single power supply A second UV lamp is required 7 Turn on the UV lamp to digest the pre...

Page 343: ...form Steps 12 15 within three minutes after the timer beeps 13 Press ZERO The cursor will move to the right then the display will show 0 0 mg L PO4 Note If Reagent Blank Correction is on the display m...

Page 344: ...check the UV conversion of phosphonate to orthophosphate Interferences When testing a 5 mL sample volume the following may interfere when present in concentrations exceeding those listed below The int...

Page 345: ...ophosphate during the UV digestion Both the sample and the blank will develop color if orthophosphate is present in the sample The increase in color in the sample is proportional to the phosphate prod...

Page 346: ...bulb 1 each 14651 00 Sample Cell 10 20 25 mL w cap 2 6 pkg 24019 06 UV Lamp with power supply 115 V with goggles 1 each 20828 00 OR UV Lamp with power supply 230 V 1 each 20828 02 OPTIONAL REAGENTS H...

Page 347: ...od Press PRGM The display will show PRGM Note For most accurate results perform a Reagent Blank Correction using deionized water see Section 1 2 Press 79 ENTER The display will show mg L PO4 and the Z...

Page 348: ...nstrument cap 8 Press ZERO The cursor will move to the right then the display will show 0 00 mg L PO4 Note If Reagent Blank Correction is on the display may flash limit See Section 1 9 After the timer...

Page 349: ...ZERO icon Note For alternate forms P P2O5 press the CONC key 3 Fill a sample cell the blank with at least 10 mL of sample Collect at least 40 mL of sample in a 50 mL beaker Note For samples with extr...

Page 350: ...persulfate digestion 7 Place the blank into the cell holder Tightly cover the sample cell with the instrument cap 8 Press ZERO The cursor will move to the right then the display will show 0 00 mg L P...

Page 351: ...of standard respectively to the three mixing cylinders Stopper each and mix thoroughly d For analysis with AccuVacs transfer solutions to dry clean 50 mL beakers to fill the AccuVac ampules For analys...

Page 352: ...ybdenum blue color Interfering Substance Interference Levels and Treatments Aluminum Greater than 200 mg L Arsenate All levels Chromium Greater than 100 mg L Copper Greater than 10 mg L Hydrogen sulfi...

Page 353: ...N 100 mL MDB 2450 32 Wastewater Effluent Standard Inorganic NH3 N NO3 N PO4 COD SO4 TOC 500 mL 28332 49 Water deionized 4 L 272 56 OPTIONAL APPARATUS AccuVac Snapper Kit each 24052 00 Ampule Breaker...

Page 354: ...354...

Page 355: ...onized water Do not use detergents containing phosphates to clean glassware Note Adjust the pH of stored samples before digestion 2 Add the contents of one Potassium Persulfate Powder Pillow Swirl to...

Page 356: ...or any color or turbidity destroyed by this procedure For alkaline or highly buffered samples it may be necessary to add additional acid in Step 3 to drop the pH of the solution below 1 5 Cool the sam...

Page 357: ...EPA approved for NPDES reporting The following reagents and apparatus are required in addition to those required for the reactive phosphorus test REQUIRED REAGENTS Quantity Required Description PerTe...

Page 358: ...67 01 Hot Plate 4 diameter 240 Vac each 12067 02 Pads cooling 4 x 4 each 18376 00 pH Indicator Paper 1 to 11 pH 5rolls pkg 391 33 pH Meter Sension 1 portable with electrode each 51700 10 For Technical...

Page 359: ...acid Rinse with deionized water Do not use detergents containing phosphate to clean glassware 2 Add 2 0 mL of 5 25 N Sulfuric Acid Solution Note Use the 1 mL calibrated dropper provided 3 Place the fl...

Page 360: ...to 25 mL Proceed with the appropriate reactive phosphorus test Note Results of the reactive phosphorus test at this point will include the orthophosphate plus the acid hydrolyzable condensed phosphate...

Page 361: ...teps to convert condensed phosphate forms meta pyro or other polyphosphates to reactive orthophosphate before analysis The procedure uses acid and heat to hydrolyze the sample Organic phosphates are n...

Page 362: ...nmeyer 50 mL 1 each 505 41 OPTIONAL REAGENTS Hydrochloric Acid 6 N 500mL 884 49 Water deionized 4L 272 56 OPTIONAL APPARATUS Cylinder graduated 50 mL each 508 41 Flask erlenmeyer 125 mL each 505 43 Ho...

Page 363: ...display will show mg L PO4 and the ZERO icon Note For alternate forms P P2O5 press the CONC key 3 Insert the COD TNT Adapter into the cell holder by rotating the adapter until it drops into place The...

Page 364: ...the first sample Read the remaining samples after adding the PhosVer 3 Reagent 9 Using a funnel add the contents of one PhosVer 3 Phosphate Powder Pillow to the vial 10 Cap the vial tightly and shake...

Page 365: ...an glassware with 1 1 hydrochloric acid solution Rinse again with deionized water Do not use detergents containing phosphates to clean glassware Standard Additions Method a Fill three 25 mL graduated...

Page 366: ...2 mL of solution from a Phosphate Voluette Ampule Standard for Phosphate 50 mg L as PO4 3 into an acid washed Class A 100 mL volumetric flask Dilute to the mark with deionized water Substitute this s...

Page 367: ...ulfide 6 mg L Sulfide interference may be removed by oxidation with Bromine Water as follows 1 Measure 25 mL of sample into a 50 mL beaker 2 Swirling constantly add Bromine Water drop wise until a per...

Page 368: ...ch 25843 35 Pipet TenSette 1 to 10 mL 1 each 19700 10 Pipet Tips for 19700 10 TenSette Pipet 1 50 pkg 21997 96 Test Tube Rack 1 3 each 18641 00 OPTIONAL REAGENTS Bromine Water 30 g L 29 mL 2211 20 Dri...

Page 369: ...umetric Class A 100 mL each 14574 42 pH Indicator Paper 1 to 11 pH units 5 rolls pkg 391 33 pH Meter sension 1 portable with electrode each 51700 10 Pipet TenSette 0 1 to 1 0 mL each 19700 01 Pipet Ti...

Page 370: ...370...

Page 371: ...mg L PO4 and the ZERO icon Note For alternate forms P P2O5 press the CONC key 4 Insert the COD TNT Adapter into the cell holder by rotating the adapter until it drops into place Then push down to ful...

Page 372: ...m each reading 12 Remove the cap from the vial Using a funnel add the contents of one PhosVer 3 Phosphate Reagent Powder Pillow to the vial 13 Cap tightly and shake for 10 15 seconds Note The powder w...

Page 373: ...th 1 1 hydrochloric acid solution Rinse with deionized water Do not use detergents containing phosphate to clean glassware Standard Additions Method a Fill three 25 mL graduated mixing cylinders with...

Page 374: ...ark with deionized water Substitute this standard for the sample and perform the procedure as described Interferences The following may interfere when present in concentrations exceeding those listed...

Page 375: ...orms meta pyro or other polyphosphates must be converted to reactive orthophosphate before analysis Pretreatment of the sample with acid and heat provides the conditions for hydrolysis of the condense...

Page 376: ...TV082 52 40001 Funnel micro 1 each 25843 35 Pipet TenSette 1 to 10 mL 1 each 19700 10 Pipet Tips for 19700 10 TenSette Pipet 50 pkg 21997 96 Test Tube Rack 1 3 each 18641 00 OPTIONAL REAGENTS Bromine...

Page 377: ...82 52 30001 Flask volumetric Class A 100 mL each 14574 42 pH Indicator Paper 1 to 11 pH units 5 rolls pkg 391 33 pH Meter sension 1 portable with electrode each 51700 10 Pipet TenSette 0 1 1 0 mL each...

Page 378: ...378...

Page 379: ...ost accurate results perform a Reagent Blank Correction using deionized water see Section 1 3 Press 82 ENTER The display will show mg L PO4 and the ZERO icon Note For alternate forms P P2O5 press the...

Page 380: ...the top of the vial until it seats solidly into the adapter Note Do not move the vial from side to side as this can cause errors 13 Tightly cover the vial with the instrument cap 14 Press ZERO The cu...

Page 381: ...seats solidly into the adapter Note Do not move the vial from side to side as this can cause errors 20 Tightly cover the vial with the instrument cap 21 Press READ The cursor will move to the right t...

Page 382: ...s with 25 mL of sample b Snap the neck off a Phosphate PourRite Ampule Standard 50 mg L as PO4 3 c Use the TenSette Pipet to add 0 1 mL 0 2 mL and 0 3 mL respectively to the three 25 mL aliquots of sa...

Page 383: ...tions exceeding those listed below Store PhosVer 3 Reagent Powder Pillows in a cool dry environment Substance Interference Level and Treatment Aluminum 200 mg L Arsenate Interferes at any level Chromi...

Page 384: ...ing an intense molybdenum blue color REQUIRED REAGENTS Total Phosphorus Test N Tube Reagent Set 50 tests 27426 45 Includes 1 272 42 1 20847 66 1 21060 46 1 27430 42 50 Acid Dilution Vials Quantity Req...

Page 385: ...it each 21968 00 Ampule Breaker PourRite ampules each 24846 00 DRB 200 Reactor 110 V 21 x 16 mm and 4 x 20 mm LTV082 53 42001 DRB 200 Reactor 220 V 21 x 16 mm and 4 x 20 mm LTV082 52 42001 DRB 200 Rea...

Page 386: ...386...

Page 387: ...er for reactive phosphate PO4 3 amino acid method Press PRGM The display will show PRGM Note For most accurate results perform a Reagent Blank Correction using deionized water see Section 1 2 Press 85...

Page 388: ...A 10 minute reaction period will begin Note Perform Step 7 while the timer is running 7 Pour 25 mL of sample the blank into a sample cell 8 When the timer beeps the display will show mg L PO4 Place th...

Page 389: ...mg L phosphate standard by pipetting 10 0 mL of a Phosphate Standard Solution 50 mg L as PO4 3 into a 50 mL volumetric flask Dilute to volume with deionized water Or prepare a 10 0 mg L PO4 3 standar...

Page 390: ...of phosphate increases the color changes from blue to green then to yellow and finally to brown The brown color may suggest a concentration as high as 100 000 mg L PO4 3 If a color other than blue is...

Page 391: ...r 30 g L 29mL 2211 20 Hydrochloric Acid Solution 1 1 6 N 500mL 884 49 Phenol Solution 30 g L 29mL 2112 20 Phosphate Standard Solution 50 mg L PO4 3 500mL 171 49 Phosphate Standard Solution PourRite am...

Page 392: ...Indicator Paper 1 to 11 pH 5rolls pkg 391 33 pH Meter sension 1 portable with electrode each 51700 10 Pipet serological 2 0 mL each 532 36 Pipet TenSette 0 1 to 1 0 mL each 19700 01 Pipet Tips for 197...

Page 393: ...re is 10 C 50 F wait 8 minutes If the sample temperature is 30 C 86 F wait 2 minutes 6 After the timer beeps add the contents of one Citric Acid Reagent Powder Pillow to each sample cell Swirl to mix...

Page 394: ...the sample cell with the instrument cap 11 Press ZERO The cursor will move to the right then the display will show 0 00 mg L SiO2 12 Place the sample into the cell holder Tightly cover the sample cell...

Page 395: ...the reading obtained with the 1 00 mg L Standard Solution see Optional Reagents press the SETUP key and scroll using the arrow keys to the STD setup option Press ENTER to activate the standard adjust...

Page 396: ...Phosphate Phosphate does not interfere at levels less than 50 mg L PO4 At 60 mg L PO4 an interference of 2 occurs At 75 mg L PO4 the interference is 11 Iron Large amounts of iron interfere Slow reacti...

Page 397: ...5 31 Sodium Bicarbonate ACS 454 g 776 01 Sodium Hydroxide Standard Solution 1 000 N 900 mL 1045 53 Sulfuric Acid Standard Solution 1 0 N 1000 mL 1270 53 OPTIONAL APPARATUS Bottle 118 mL polyethylene o...

Page 398: ...398...

Page 399: ...should be 15 to 25 C 59 to 77 F 4 Fill both sample cells to the 25 mL line with deionized water Set one sample cell aside as the blank 5 To the other cell add the contents of one Molybdate Reagent Pow...

Page 400: ...or will move to the right then the display will show 0 mg L SiO2 Note If Reagent Blank Correction is on the display may flash limit See Section 1 12 Place the prepared sample into the cell holder Tigh...

Page 401: ...g L silica standard pipet 40 0 mL of a 1000 mg L Silica Standard Solution into a 250 mL volumetric flask Dilute to the line with deionized water Analyze according to the above procedure using deionize...

Page 402: ...ore adding citric acid may help in lieu of the bicarbonate treatment Summary of Method Silica and phosphate in the sample react with molybdate ion under acidic conditions to form yellow silicomolybdic...

Page 403: ...L 236 mL 21225 31 Silica Standard Solution 50 mg L 200 mL 1117 29 Silica Standard Solution 1000 mg L 500 mL 194 49 Sodium Bicarbonate ACS 454 g 776 01 Sulfuric Acid Standard Solution 1 000 N 100 mL M...

Page 404: ...404...

Page 405: ...n at the back of this procedure Program 91 can be used for process control or applications where a high degree of accuracy is not needed Note The nature of turbidimetric tests and reagent lot variatio...

Page 406: ...ell with 10 mL of sample the blank 8 Place the blank into the cell holder Tightly cover the sample cell with the instrument cap 9 Press ZERO The cursor will move to the right then the display will sho...

Page 407: ...t least 40 mL of sample in a 50 mL beaker Note Filter highly turbid or colored samples Use filtered sample in this step and as the blank 5 Fill a SulfaVer 4 Sulfate AccuVac Ampul with sample Note Keep...

Page 408: ...ate standard into 100 mL volumetric flasks Dilute to the mark with deionized water and mix well Zero the instrument with water The user entered settings for sulfate are Program number 101 to 105 Wavel...

Page 409: ...d PourRite Ampule 2500 mg L SO4 2 b Fill three 25 mL graduated cylinders with 25 mL of sample Use a TenSette Pipet to add 0 1 0 2 and 0 3 mL of standard to the three cylinders Mix thoroughly For AccuV...

Page 410: ...dard deviation of 0 5 mg L sulfate In a single laboratory using a standard solution of 50 mg L sulfate and two representative lots of AccuVac Ampuls with the instrument a single operator obtained a st...

Page 411: ...Rite Ampule 1000 mg L 2 mL 20 pkg 21757 20 Water deionized 4 L 272 56 OPTIONAL APPARATUS AccuVac Snapper Kit each 24052 00 Cylinder graduated mixing 25 mL each 20886 40 Filter Paper folded 12 5 cm 100...

Page 412: ...412...

Page 413: ...d cannot be preserved for later analysis Use a pipet to avoid agitation Note For field testing a 25 mL graduated cylinder may be used 4 Fill a second sample cell with 25 mL of deionized water the blan...

Page 414: ...erator obtained a standard deviation of 0 02 mg L sulfide Estimated Detection Limit EDL The EDL for program 93 is 0 01 mg L S2 For more information on derivation and use of Hach s estimated detection...

Page 415: ...ncentration regulated as a hazardous waste by Federal RCRA See Section 3 for more information on proper disposal of these materials Interfering Substance Interference Levels and Treatments Strong redu...

Page 416: ...safety bulb 1 each 14651 00 Sample Cell 10 20 25 mL w cap 2 6 pkg 24019 06 OPTIONAL REAGENTS Description Units Cat No Bromine Water 30 g L 29 mL 2211 20 Phenol Solution 30 g L 29 mL 2112 20 Sodium Su...

Page 417: ...five seconds 5 Add the contents of one Detergents Reagent Powder Pillow to the funnel Stopper the funnel and shake to dissolve the powder 6 Add 30 mL of benzene to the funnel Stopper the funnel and s...

Page 418: ...ell to the 25 mL mark with pure benzene the blank 12 Place the blank in the cell holder Tightly cover the sample cell with the instrument cap 13 Press ZERO The cursor will move to the right then the d...

Page 419: ...If these increases do not occur see Standard Additions Section 1 for more information Method Performance Precision In a single laboratory using a standard solution of 0 150 mg L LAS two lots of reagen...

Page 420: ...aduated 25 mL 1 each 508 40 Cylinder graduated 50 mL 1 each 508 41 Cylinder graduated 500 mL 1 each 508 49 Funnel separatory 500 mL 1 each 520 49 Ring support 4 inch 1 each 580 01 Sample Cell 10 20 25...

Page 421: ...in a blender at high speed for exactly 2 minutes 4 Pour the blended sample into a 600 mL beaker 5 Fill a sample cell with 25 mL of tap water or deionized water the blank Note Remove gas bubbles in th...

Page 422: ...tection limit see Section 1 Interferences Calibration for this test is based on parallel samples using the gravimetric technique on sewage samples from a municipal sewage plant For most samples this c...

Page 423: ...S Quantity Required Description Per Test Unit Cat No Beaker 600 mL low form 1 each 1080 52 Blender 1 2 L 120 V each each 26161 00 Blender 1 2 L 240 V each each 26161 02 Cylinder graduated 500 mL poly...

Page 424: ...424...

Page 425: ...mL mark with sample the prepared sample Note Filter turbid samples and report results as mg L soluble tannic acid 5 Pipet 0 5 mL of TanniVer 3 Tannin Lignin Reagent into each cell Swirl to mix 6 Pipe...

Page 426: ...id and two representative lots of reagent with the instrument a single operator obtained a standard deviation of 0 1 mg L tannic acid Estimated Detection Limit The estimated detection limit for progra...

Page 427: ...Water deionized 25 mL 4 L 272 56 REQUIRED APPARATUS Pipet Filler safety bulb 1 each 14651 00 Pipet volumetric Class A 5 0 mL 1 each 14515 37 Pipet volumetric Class A 0 5 mL 1 each 14515 34 Sample Cel...

Page 428: ...67 Pipet TenSette 0 1 to 1 0 mL each 19700 01 Pipet Tips for 19700 01 Pipet 50 pkg 21856 96 Pipet Tips for 19700 01 Pipet 1000 pkg 21856 28 Pipet volumetric Class A 10 00 mL each 14515 38 Pipet Filler...

Page 429: ...with an E coli Aqua QC Stik according to the instructions that come with the stick 2 Incubate the Lauryl Tryptose Broth Tube at 35 C 95 F until the medium is visibly turbid approxamately 12 hours Turb...

Page 430: ...band should NOT be removed 4 Fill a Test N Tube vial with deionized water Label this vial as the blank Wipe the outside of all the vials with a tissue to remove fingerprints and smudges 5 Place the bl...

Page 431: ...rt to mix 12 Add 0 5 mL of inoculum previously prepared to each vial Cap and invert to mix 13 Place the control vial in the cell holder Tightly cover the vial with the instrument cap 14 Press READ The...

Page 432: ...ach absorbance value 21 Calculate the Inhibition as follows A is the initial absorbance value minus the final absorbance value See the example following this step Note Some toxins increase respiration...

Page 433: ...s look at the series of data to determine the likelihood of toxicity Results below 10 are not reliable but can be used to surmise some presence of toxicity if they are consistent See the table below S...

Page 434: ...EQUIRED REAGENTS Description Cat No ToxTrak Reagent Set 25 tests 25972 00 Includes 1 25607 66 1 25608 36 1 22777 00 1 24092 32 Quantity Required Description Per Test Unit Cat No Aqua QC Stiks Escheric...

Page 435: ...Dri Bath 25 well 120 230 V each 45900 00 Incubator Dri Bath 25 well 120 230 V with European power cord each 45900 02 Pipet Sterile Transfer 15 pkg 22325 12 Timer each 26305 00 For Technical Assistanc...

Page 436: ...436...

Page 437: ...a soft cloth Note For highly colored samples use a filtered portion of sample in place of the deionized water 4 Place the blank into the cell holder Tightly cover the sample cell with the instrument...

Page 438: ...rbidity stock solution 200 NTU StablCal Standard is available from Hach Standard Adjust To adjust the calibration curve using the reading obtained with the 200 FAU formazin standard press the SETUP ke...

Page 439: ...ent for FAU is very different than the NTU method 1 NTU 1 FTU 1 FAU when traced to formazin primary standards REQUIRED APPARATUS Quantity Required Description Per Test Unit Cat No Sample Cell 10 20 25...

Page 440: ...Oiling cloth for applying silicone oil each 26873 00 Pipet Filler safety bulb each 14651 00 Pipet volumetric Class A 5 0 mL each 14515 37 Sample Degassing Kit each 43975 00 Stopper rubber one hole No...

Page 441: ...as described in the Hach Distillation Apparatus manual 3 Pipet 0 5 mL of deionized water into a dry 25 mL sample cell the blank Note Use a Class A or TenSette Pipet Note Adjust the pH of stored sampl...

Page 442: ...olution into each cell Cap and invert to mix 13 Add 10 mL of Ferric Chloride Sulfuric Acid Solution to each cell Cap and invert to mix 14 Add 10 mL of deionized water to each cell Cap and invert to mi...

Page 443: ...liquot of sample from each cylinder add to three dry sample cells Analyze all three samples along with the original test sample beginning with Step 5 of the procedure The volatile acid concentration s...

Page 444: ...1 Summary of Method The volatile acids test is designed specifically for the determination of volatile acids in digestor sludges The method is based on esterification of the carboxylic acids present...

Page 445: ...TUS Ampule Breaker PourRite each 24846 00 Beaker 600 mL each 500 52 Bottle wash 500 mL each 620 11 Centrifuge laboratory 115 Vac each 26765 00 Centrifuge laboratory 230 Vac each 26765 02 Centrifuge Tu...

Page 446: ...446...

Page 447: ...following these steps 3 Fill a 25 mL sample cell with 20 mL of sample Note Rinse glassware with 1 1 hydrochloric acid and deionized water before use Note If samples cannot be analyzed immediately see...

Page 448: ...riod will begin Note Steps 9 11 must be completed within 10 minutes after the timer beeps 9 Place the blank into the cell holder Tightly cover the sample cell with the instrument cap 10 Press ZERO The...

Page 449: ...es Mix each thoroughly c Analyze each sample as described above The zinc concentration should increase 0 1 mg L for each 0 1 mL of standard added d If these increases do not occur see Standard Additio...

Page 450: ...aratus b While stirring add the waste to a beaker containing a strong solution of sodium hydroxide and calcium hypochlorite or sodium hypochlorite household bleach c Maintain a strong excess of hydrox...

Page 451: ...cap 2 6 pkg 24019 06 Squeezers plastic dropper 1 20 pkg 21247 20 OPTIONAL REAGENTS Bleach household 1 gal buy locally Cylinder graduated mixing 25mL each 20886 40 Hydrochloric Acid Standard Solution 6...

Page 452: ...erological 2 mL each 532 36 Pipet TenSette 0 1 to 1 0 mL each 19700 01 Pipet TenSette tips for 19700 01 50 pkg 21856 96 Pipet TenSette 1 0 to 10 0 mL each 19700 10 Pipet TenSette tips for 19700 01 100...

Page 453: ...ber if available Billing address Shipping address Your name and phone number Purchase order number Catalog number Brief description or model number Quantity Technical and Customer Service Hach Technic...

Page 454: ...the shipping point usually Ames Iowa Hach offers instant credit up to 200 on Net 30 Day terms Larger orders are subject to credit review Customers may send remittance with orders or we can ship C O D...

Page 455: ...ders for safe arrival Unless we are instructed otherwise the best and most efficient mode of transportation is selected Motor freight shipments will be sent freight collect unless you specify otherwis...

Page 456: ......

Page 457: ...documentation identifying your tax exempt number If taxable sales tax will be added MAIL ORDER FORM Send order to HACH COMPANY P O Box 608 Loveland CO 80539 0608 Use this convenient form your own purc...

Page 458: ...Shipping Charge Prices are subject to change without notice TAXABLE Yes No If no tax exempt document is Enclosed On file at Hach TOTAL ORDER QUANTIT Y CAT NO DESCRIPTION UNIT SIZE UNIT PRICE TOTAL...

Page 459: ......

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