DR/890 COLORIMETER PROCEDURES MANUAL

1 48470-22DR/890 COLORIMETERPROCEDURES MANUAL Hach Company, 1997-2009. All rights reserved. Printed in the te/dk 2/09 9ed1 TABLE OF 7 Sample Procedure Explained ..9 SECTION 1 CHEMICAL ANALYSIS 13 Abbreviations .. 13 Converting Chemical Species .. 14 Hardness Conversion .. 15 Dissolved 16 Sample Collection, Preservation and 18 Collecting Water Samples ..21 acid Washing Bottles ..22 Correcting for Volume Additions .. 22 Boiling 23 Sample Filtration .. 23 Temperature Considerations .. 25 Sample Dilution 25 Using Pipets and Graduated Cylinders .. 26 Using the TenSette 28 Mixing Water Samples .. 29 Using Sample 31 Orientation of Sample of Hach Sample Cells ..31 Cleaning Sample Cells ..31 Using the COD/TNT Adapter ..31 Volume Measurement Using AccuVac 32 Using Reagent Powder Pillows.

2 33 Using PermaChem Pillows .. 33 Reagent and Standard 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).. 472 TABLE OF CONTENTS, continued Preparing a User-Entered Calibration Curve .. 49%T Versus Concentration Calibration ..49 Absorbance Versus Concentration USEPA Approved and Accepted Definitions .. 51 SECTION 2 SAMPLE 53 Digestion .. 53 EPA Mild Digestion with Hot Plate for Metals Analysis 53 EPA Vigorous Digestion with Hot Plate for Metals Analysis 54 General Digesdahl Digestion (Not USEPA accepted) .. 55 Distillation .. 55 SECTION 3 WASTE MANAGEMENT AND 57 Waste Management.

3 57 Waste Minimization .. 57 Regulatory Overview .. 57 Hazardous Waste 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 Resources .. 62 Material Safety Data 63 How to Obtain an MSDS .. 63 Sections of the MSDS .. 63 Safety .. 66 Material Safety Data 66 Reading Labels 66 Protective Equipment .. 66 First Aid Equipment and Supplies .. 67 General Safety Rules .. 67 OSHA Chemical Hygiene Plan .. 68 SECTION 4 69 ALUMINUM, Aluminon Method .. 71 BENZOTRIAZOLE, or TOLYLTRIAZOLE, UV Photolysis Method .. 77 BROMINE, DPD 833 TABLE OF CONTENTS, continuedCHLORAMINE, MONO, Low Range, CHLORAMINE, MONO, High Range, Indophenol Method.

4 99 CHLORINE DIOXIDE, DPD 107 CHLORINE DIOXIDE, Mid Range, Direct Reading Method .. 115 CHLORINE, FREE, Ultra-high Range, DPD 117 CHLORINE, TOTAL, Ultra-High Range, DPD 125 CHLORINE, FREE, DPD Method .. 133 CHLORINE, TOTAL, DPD Method .. 141 CHLORINE, FREE, DPD Test N Tube 149 CHLORINE, TOTAL, DPD Test N Tube 155 CHROMIUM, HEXAVALENT, 1,5-Diphenylcarbohydrazide Method .. 161 CHROMIUM, TOTAL, Alkaline Hypobromite Oxidation Method .. 167 COLOR, TRUE AND APPARENT, APHA Platinum-Cobalt Standard Method .. 173 COPPER, Bicinchoninate Method .. 177 COPPER, Porphyrin Method .. 187 CYANIDE, Pyridine-Pyrazalone Method .. 193 CYANURIC acid , Turbidimetric Method .. 203 DEHA, Iron Reduction Method for Oxygen 207 FLUORIDE, SPADNS 211 FLUORIDE, SPADNS 2 219 HARDNESS, Calcium and Magnesium; Calmagite Colorimetric Method.

5 227 HYDRAZINE, p-Dimethylaminobenzaldehyde 231 IRON, FERROUS, 1,10 Phenanthroline Method .. 237 IRON, TOTAL, FerroVer 243 IRON, FerroZine 251 IRON, TOTAL, FerroMo 257 IRON, TOTAL, TPTZ Method .. 261 MANGANESE, High Range, Periodate Oxidation Method .. 269 MANGANESE, Low Range, PAN Method .. 273 MOLYBDENUM, MOLYBDATE, Low Range, Ternary Complex Method .. 279 MOLYBDENUM, MOLYBDATE, High Range, Mercaptoacetic acid 285 Nitrogen, Free Ammonia and Chloramine (Mono), Indophenol Method .. 291 NICKEL, PAN Method .. 301 NITRATE, High Range, Cadmium Reduction Method .. 305 NITRATE, Mid Range, Cadmium Reduction 313 NITRATE, Low Range, Cadmium Reduction Method .. 3214 TABLE OF CONTENTS, continuedNITRATE, High Range, Test N Tube, , Chromotropic acid Method .. 327 NITRITE, High Range, Ferrous Sulfate 333 NITRITE, Low Range, Diazotization Method.

6 337 NITRITE, Low Range, Test N Tube, Diazotization Method .. 343 NITROGEN, AMMONIA, Salicylate 347 NITROGEN, TOTAL KJELDAHL, Nessler Method .. 353 NITROGEN, AMMONIA, Low Range, Test N Tube, Salicylate Method .. 361 NITROGEN, AMMONIA, High Range, Test N Tube, Salicylate 367 NITROGEN, Total Inorganic, Test N Tube , Titanium Trichloride Reduction Method .. 373 NITROGEN, TOTAL, Test N Tube, TNT Persulfate Digestion 381 NITROGEN, TOTAL, HR, Test N Tube , TNT Persulfate Digestion Method .. 391 ORGANIC CARBON, TOTAL, Low Range, Direct 401 ORGANIC CARBON, TOTAL, Mid Range, Direct Method .. 409 ORGANIC CARBON, TOTAL, High Range, Direct Method .. 417 OXYGEN DEMAND, CHEMICAL, Reactor Digestion 425 Colorimetric Determination, 0 to 150 mg/L 427 Colorimetric Determination, 0 to 1,500 and 0 to 15,000 mg/L 428 OXYGEN DEMAND, CHEMICAL, Manganese III Digestion Method.

7 435 OXYGEN DEMAND, CHEMICAL, Manganese III Digestion Method .. 441 OXYGEN, DISSOLVED, High Range, HRDO 451 OXYGEN, DISSOLVED, Low Range, Indigo Carmine 455 OZONE, Indigo Method .. 459pH, Colorimetric pH Determination Using Phenol Red .. 463 PHOSPHONATES, Persulfate UV Oxidation 467 PHOSPHORUS, REACTIVE, (Also called Orthophosphate) PhosVer 3 (Ascorbic acid ) Method .. 473 PHOSPHORUS, REACTIVE, PhosVer 3 Method, Test N Tube 481 PHOSPHORUS, REACTIVE, Amino acid Method .. 489 PHOSPHORUS, REACTIVE, (Also called Orthophosphate) Molybdovanadate Method .. 495 PHOSPHORUS, REACTIVE, HR, Molybdovanadate Method, Test N Tube Procedure .. 503 PHOSPHORUS, acid HYDROLYZABLE, Hydrolysis to Orthophosphate Method .. 511 PHOSPHORUS, acid HYDROLYZABLE, PhosVer 3 with acid 515 PHOSPHORUS, TOTAL, (Also called Organic and acid Hydrolyzable) acid Persulfate Digestion Method.

8 523 PHOSPHORUS, TOTAL, PhosVer 3 with acid Persulfate Digestion .. 5275 TABLE OF CONTENTS, continuedPHOSPHORUS, TOTAL, HR, Molybdovanadate Method with acid Persulfate Digestion Test N Tube Procedure .. 535 SILICA, Low Range, Heteropoly Blue Method .. 545 SILICA, High Range, Silicomolybdate Method .. 551 SILICA, Ultra High Range, Silicomolybdate Method .. 555 SULFATE, SulfaVer 4 561 SULFIDE, Methylene Blue Method .. 569 SURFACTANTS, ANIONIC, (Also called: Detergents) Crystal Violet Method .. 573 SUSPENDED SOLIDS, Photometric 577 TANNIN AND LIGNIN, Tyrosine Method .. 581 TOXTRAK TOXICITY TEST, Colorimetric 585 TURBIDITY, Absorptometric Method .. 593 VOLATILE ACIDS, Esterification 597 ZINC, Zincon 603 HOW TO ORDER .. 609 ADDITIONAL INFORMATION .. 61167 INTRODUCTIONThis MANUAL is divided into five sections:Section 1 Chemical Analysis Information This section applies to all the PROCEDURES .

9 It provides background information and reference/review material for the technician or chemist. Commonly used techniques are explained in 2 Sample PretreatmentThis 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 3 Waste Management and SafetySection 3 includes information on waste management, regulations, waste disposal and resources on waste management. The Safety portion covers reading an MSDS and general safety 4 ProceduresSection 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 5 Ordering InformationThis section provides information needed for ordering, shipping, return of items and Hach attempting the analysis PROCEDURES the analyst should read the instrument MANUAL to learn about the COLORIMETER s features and Procedure Explained10 Sample Procedure Explained, continued11 Sample Procedure Explained, continued12 Sample Procedure Explained, continued13 SECTION 1 CHEMICAL ANALYSIS INFORMATIONA bbreviationsThe following abbreviations are used throughout the text of the procedure section.

10 Abbrev-iationDefinitionAbbrev-iationDefi nition Cdegree(s) Celsius (Centigrade)MDLM ethod detection limit Fdegree(s) FahrenheitMDBmarked dropping bottleACSA merican Chemical Society reagent grade puritymg/Lmilligrams per liter (ppm)APHA Standard MethodsStandard Methods for the Examination of Water and 1 Published jointly by the American Public Health Association (APHA), the American Water Works Association (AWWA), and the Water Environment Federation (WEF). Order from Hach requesting Cat. No. 22708-00 or from the Publication Office of the American Public Health Association. This book is the standard reference work for water analysis. Many PROCEDURES contained in this MANUAL are based on Standard Methods. g/Lmicrograms per liter (ppb)AVAccuVac mL(milliliter)-approximately the same as a cubic centimeter (cc) or 1/1000 of a liter.