DR/890 COLORIMETER PROCEDURES MANUAL

616 Pages·2013·7.69 MB·English

48470-22
DR/890
COLORIMETER
PROCEDURES MANUAL
© Hach Company, 1997-2009, 2013. All rights reserved. Printed in the U.S.A. te/dk 03/13 10ed

TABLE OF CONTENTS
INTRODUCTION..................................................................................................................... 7
Sample Procedure Explained ....................................................................................................9
SECTION 1 CHEMICAL ANALYSIS INFORMATION........................................ 13
Abbreviations......................................................................................................................... 13
Converting Chemical Species................................................................................................ 14
Hardness Conversion....................................................................................................... 15
Dissolved Oxygen............................................................................................................ 16
Sample Collection, Preservation and Storage.................................................................. 18
Collecting Water Samples...........................................................................................21
Acid Washing Bottles..................................................................................................22
Correcting for Volume Additions.................................................................................... 22
Boiling Aids..................................................................................................................... 23
Sample Filtration............................................................................................................. 23
Temperature Considerations............................................................................................ 25
Sample Dilution Techniques............................................................................................ 25
Using Pipets and Graduated Cylinders............................................................................ 26
Using the TenSette Pipet.................................................................................................. 28
Mixing Water Samples.................................................................................................... 29
Using Sample Cells.......................................................................................................... 31
Orientation of Sample Cells.........................................................................................31
Care of Hach Sample Cells..........................................................................................31
Cleaning Sample Cells.................................................................................................31
Using the COD/TNT Adapter......................................................................................31
Volume Measurement Accuracy..................................................................................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
Standard Additions.......................................................................................................... 36
Method Performance.............................................................................................................. 43
Estimated Detection Limit............................................................................................... 43
Precision.......................................................................................................................... 46
Estimating Precision....................................................................................................46
Reagent Blank Correction...................................................................................................... 47
Standard Adjust (Adjusting the Standard Curve)................................................................... 47
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TABLE OF CONTENTS, continued
Preparing a User-Entered Calibration Curve.................................................................. 49
%T Versus Concentration Calibration.........................................................................49
Absorbance Versus Concentration Calibration............................................................51
USEPA Approved and Accepted Definitions........................................................................ 51
SECTION 2 SAMPLE PRETREATMENT................................................................. 53
Digestion................................................................................................................................ 53
EPA Mild Digestion with Hot Plate for Metals Analysis Only....................................... 53
EPA Vigorous Digestion with Hot Plate for Metals Analysis Only................................ 54
General Digesdahl Digestion (Not USEPA accepted).................................................... 55
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
Special Considerations for Cyanide-Containing Materials..........................................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
BENZOTRIAZOLE, or TOLYLTRIAZOLE, UV Photolysis Method.................................. 77
BROMINE, DPD Method....................................................................................................... 83
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TABLE OF CONTENTS, continued
CHLORAMINE, MONO, Low Range, CHLORAMINE, MONO, High Range, Indophenol
Method.............................................................................................................................. 99
CHLORINE DIOXIDE, DPD Method.................................................................................. 107
CHLORINE DIOXIDE, Mid Range, Direct Reading Method............................................. 115
CHLORINE, FREE, Ultra-high Range, DPD Method.......................................................... 117
CHLORINE, TOTAL, Ultra-High Range, DPD Method...................................................... 125
CHLORINE, FREE, DPD Method....................................................................................... 133
CHLORINE, TOTAL, DPD Method.................................................................................... 141
CHLORINE, FREE, DPD Test ‘N Tube™ Method.............................................................. 149
CHLORINE, TOTAL, DPD Test ‘N Tube™ Method........................................................... 157
CHROMIUM, HEXAVALENT, 1,5-Diphenylcarbohydrazide Method............................... 163
CHROMIUM, TOTAL, Alkaline Hypobromite Oxidation Method ................................... 169
COLOR, TRUE AND APPARENT, APHA Platinum-Cobalt Standard Method................. 175
COPPER, Bicinchoninate Method........................................................................................ 179
COPPER, Porphyrin Method................................................................................................ 189
CYANIDE, Pyridine-Pyrazalone Method............................................................................. 195
CYANURIC ACID, Turbidimetric Method.......................................................................... 205
DEHA, Iron Reduction Method for Oxygen Scavengers...................................................... 209
FLUORIDE, SPADNS Method............................................................................................. 213
FLUORIDE, SPADNS 2 Method.......................................................................................... 221
HARDNESS, Calcium and Magnesium; Calmagite Colorimetric Method.......................... 229
HYDRAZINE, p-Dimethylaminobenzaldehyde Method...................................................... 233
IRON, FERROUS, 1,10 Phenanthroline Method................................................................. 239
IRON, TOTAL, FerroVer Method......................................................................................... 245
IRON, FerroZine Method...................................................................................................... 253
IRON, TOTAL, FerroMo™ Method...................................................................................... 259
IRON, TOTAL, TPTZ Method............................................................................................. 263
MANGANESE, High Range, Periodate Oxidation Method................................................. 271
MANGANESE, Low Range, PAN Method.......................................................................... 275
MOLYBDENUM, MOLYBDATE, Low Range, Ternary Complex Method........................ 281
MOLYBDENUM, MOLYBDATE, High Range, Mercaptoacetic Acid Method.................. 287
Nitrogen, Free Ammonia and Chloramine (Mono), Indophenol Method............................. 293
NICKEL, PAN Method......................................................................................................... 303
NITRATE, High Range, Cadmium Reduction Method........................................................ 307
NITRATE, Mid Range, Cadmium Reduction Method.......................................................... 315
NITRATE, Low Range, Cadmium Reduction Method......................................................... 323
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TABLE OF CONTENTS, continued
NITRATE, High Range, Test ‘N Tube, , Chromotropic Acid Method................................. 329
NITRITE, High Range, Ferrous Sulfate Method.................................................................. 335
NITRITE, Low Range, Diazotization Method..................................................................... 339
NITRITE, Low Range, Test ‘N Tube, Diazotization Method.............................................. 345
NITROGEN, AMMONIA, Salicylate Method..................................................................... 349
NITROGEN, TOTAL KJELDAHL, Nessler Method.......................................................... 355
NITROGEN, AMMONIA, Low Range, Test ‘N Tube, Salicylate Method......................... 363
NITROGEN, AMMONIA, High Range, Test ‘N Tube, Salicylate Method......................... 369
NITROGEN, Total Inorganic, Test ‘N Tube™, Titanium Trichloride Reduction Method... 375
NITROGEN, TOTAL, Test ‘N Tube, TNT Persulfate Digestion Method............................ 383
NITROGEN, TOTAL, HR, Test ‘N Tube™, TNT Persulfate Digestion Method................ 393
ORGANIC CARBON, TOTAL, Low Range, Direct Method.............................................. 403
ORGANIC CARBON, TOTAL, Mid Range, Direct Method.............................................. 411
ORGANIC CARBON, TOTAL, High Range, Direct Method............................................. 419
OXYGEN DEMAND, CHEMICAL, Reactor Digestion Method........................................ 427
Colorimetric Determination, 0 to 150 mg/L COD................................................................ 429
Colorimetric Determination, 0 to 1,500 and 0 to 15,000 mg/L COD................................... 430
OXYGEN DEMAND, CHEMICAL, Manganese III Digestion Method............................. 437
OXYGEN DEMAND, CHEMICAL, Manganese III Digestion Method............................. 443
OXYGEN, DISSOLVED, High Range, HRDO Method...................................................... 453
OXYGEN, DISSOLVED, Low Range, Indigo Carmine Method........................................ 457
OZONE, Indigo Method....................................................................................................... 461
pH, Colorimetric pH Determination Using Phenol Red....................................................... 465
PHOSPHONATES, Persulfate UV Oxidation Method......................................................... 469
PHOSPHORUS, REACTIVE, (Also called Orthophosphate) PhosVer 3(Ascorbic Acid)
Method........................................................................................................................... 475
PHOSPHORUS, REACTIVE, PhosVer 3 Method, Test ’N Tube Procedure....................... 483
PHOSPHORUS, REACTIVE, Amino Acid Method........................................................... 491
PHOSPHORUS, REACTIVE, (Also called Orthophosphate) Molybdovanadate Method.. 497
PHOSPHORUS, REACTIVE, HR,
Molybdovanadate Method, Test ’N Tube™ Procedure................................................. 505
PHOSPHORUS, ACID HYDROLYZABLE, Hydrolysis to Orthophosphate Method........ 513
PHOSPHORUS, ACID HYDROLYZABLE, PhosVer 3 with Acid Hydrolysis.................. 517
PHOSPHORUS, TOTAL, (Also called Organic and Acid Hydrolyzable) Acid Persulfate
Digestion Method........................................................................................................... 525
PHOSPHORUS, TOTAL, PhosVer 3 with Acid Persulfate Digestion................................. 529
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TABLE OF CONTENTS, continued
PHOSPHORUS, TOTAL, HR, Molybdovanadate Method with Acid Persulfate Digestion
Test ’N Tube™ Procedure.............................................................................................. 537
SILICA, Low Range, Heteropoly Blue Method................................................................... 547
SILICA, High Range, Silicomolybdate Method................................................................... 553
SILICA, Ultra High Range, Silicomolybdate Method.......................................................... 557
SULFATE, SulfaVer 4 Method.............................................................................................. 563
SULFIDE, Methylene Blue Method..................................................................................... 571
SURFACTANTS, ANIONIC, (Also called: Detergents) Crystal Violet Method................. 575
SUSPENDED SOLIDS, Photometric Method...................................................................... 579
TANNIN AND LIGNIN, Tyrosine Method.......................................................................... 583
TOXTRAK™ TOXICITY TEST, Colorimetric Method....................................................... 587
TURBIDITY, Absorptometric Method................................................................................. 595
VOLATILE ACIDS, Esterification Method.......................................................................... 599
ZINC, Zincon Method........................................................................................................... 605
HOW TO ORDER................................................................................................................ 611
ADDITIONAL INFORMATION......................................................................................... 613
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INTRODUCTION
This manual is divided into five sections:
Section 1 Chemical Analysis Information
This section applies to all the procedures. It provides background
information and reference/review material for the technician or chemist.
Commonly used techniques are explained in detail.
Section 2 Sample Pretreatment
This section provides a brief overview of sample pretreatment and two
USEPA digestions. A brief discussion of the Hach Digesdahl Digestion
Apparatus and the Hach Distillation Apparatus is included.
Section 3 Waste Management and Safety
Section 3 includes information 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-by-step illustrated instructions for measuring
parameters. The steps also include helpful notes. Each procedure contains
information on sample collection, storage and preservation, accuracy
checks, possible interferences, summary of method and a list of the
reagents and apparatus necessary to run the test.
Section 5 Ordering Information
This section provides information needed for ordering, shipping, return of
items and Hach trademarks.
Before attempting the analysis procedures the
analyst should read the instrument manual to learn
about the colorimeter’s features and operation.
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