Page 3: Table Of Contents
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 Correcting for Volume Additions ..................22 Boiling Aids........................
Page 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 ..................
Page 5 TABLE OF CONTENTS, continued FLUORIDE, SPADNS 2 Method..................177 HARDNESS, Calcium and Magnesium; Calmagite Colorimetric Method ......185 IRON, FERROUS, 1,10 Phenanthroline Method ..............189 IRON, TOTAL, FerroVer Method..................195 ™ IRON, TOTAL, FerroMo Method..................203 IRON, TOTAL, TPTZ Method ..................... 207 MANGANESE, High Range, Periodate Oxidation Method ..........
Page 6 TABLE OF CONTENTS, continued SILICA, Low Range, Heteropoly Blue Method ..............393 SILICA, Ultra High Range, Silicomolybdate Method ............399 SULFATE, SulfaVer 4 Method ..................... 405 SULFIDE, Methylene Blue Method..................413 SURFACTANTS, ANIONIC, (Also called: Detergents) Crystal Violet Method....417 SUSPENDED SOLIDS, Photometric Method ..............
Page 7: Introduction
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.
Page 9: Sample Procedure Explained
Sample Procedure Explained...
Page 10 Sample Procedure Explained, continued...
Page 11 Sample Procedure Explained, continued...
Page 12 Sample Procedure Explained, continued...
Page 13: Section 1 Chemical Analysis Information
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...
Page 14: Converting Chemical Species
CHEMICAL ANALYSIS INFORMATION , continued Converting Chemical Species Species conversion factors for many commonly used substances are pre- programmed into the instrument (see Table 1). Conversions are method specific and are viewable after taking the reading by pressing CONC Table 1 Conversion Factors To Convert From...
Page 15: Hardness Conversion
CHEMICAL ANALYSIS INFORMATION , continued Hardness Conversion Table 2 lists the factors for converting one unit of measure for hardness to another unit of measure. For example, to convert mg/L CaCO to German parts/100,000 CaO, multiply the value in mg/L x 0.056. Table 2 Hardness Conversion Factors British gr/ America...
Page 16: Dissolved Oxygen
CHEMICAL ANALYSIS INFORMATION , continued Dissolved Oxygen Table 3 lists the mg/L dissolved oxygen in water at saturation for various temperatures and atmospheric pressures. The table was formulated in a laboratory using pure water. The values given are only approximations for estimating the oxygen content of a particular body of surface water.
Page 17 CHEMICAL ANALYSIS INFORMATION , continued Table 3 Dissolved Oxygen Saturation In Water (continued) Pressure in Millimeters and Inches Hg Temp inches °F °C 30.51 29.92 29.53 28.45 27.56 26.57 25.59 24.61 75.2 77.0 78.8 80.6 82.4 84.2 86.0 87.8 89.6 91.4 93.2 95.0...
Page 18: Sample Collection, Preservation And Storage
CHEMICAL ANALYSIS INFORMATION , continued Sample Collection, Preservation and Storage Correct sampling and storage are critical for accurate testing. For greatest accuracy, thoroughly clean sampling devices and containers to prevent carryover from previous samples. Preserve the sample properly; each procedure has information about sample preservation. •...
Page 19 CHEMICAL ANALYSIS INFORMATION , continued Table 4 Required Containers, Preservation Techniques and Holding Times Parameter No./Name Container Preservation Maximum Holding Time Table 1A - Bacterial Tests: 1-4. Coliform, fecal and total Cool, 4°C, 0.008%, Na 6 hours 5. Fecal streptococci Cool, 4°C, 0.008%, Na 6 hours Table 1B - Inorganic Tests:...
Page 20 CHEMICAL ANALYSIS INFORMATION , continued Table 4 Required Containers, Preservation Techniques and Holding Times (continued) Parameter No./Name Container Preservation Maximum Holding Time 48. Phenols G only Cool 4°C, H to pH<2 28 days 49. Phosphorus, elemental Cool, 4°C 48 hours 50.
Page 21 CHEMICAL ANALYSIS INFORMATION , continued Collecting Water Samples Obtain the best sample by careful collection. In general, collect samples near the center of the vessel or duct and below the surface. Use only clean containers (bottles, beakers). Rinse the container several times first with the water to be sampled.
Page 22: Correcting For Volume Additions
CHEMICAL ANALYSIS INFORMATION , continued Acid Washing Bottles If a procedure suggests acid-washing, use the following instructions: a) Clean the glassware or plasticware with laboratory detergent (phosphate-free detergent is recommended). b) Rinse well with tap water. c) Rinse with a 1:1 Hydrochloric Acid Solution or 1:1 Nitric Acid Solution.
Page 23: Boiling Aids
CHEMICAL ANALYSIS INFORMATION , continued Hach 1:1 Nitric Acid Pillows contain 2.5 mL of acid; correct for this volume. The addition of a Sodium Carbonate Power Pillow (neutralizes the 1:1 Nitric Acid Solution Pillow) does not need to be corrected for.
Page 24 CHEMICAL ANALYSIS INFORMATION , continued REQUIRED APPARATUS FOR VACUUM FILTRATION Description Unit Cat. No Filter Discs, glass 47 mm, 1.5 µm ............100/pkg.... 2530-00 Filter Holder, membrane................each..13529-00 Flask, filter, 500 mL..................each....546-49 Pump, vacuum, hand operated..............each..14283-00 Pump, vacuum, portable, 115 V..............
Page 25: Temperature Considerations
CHEMICAL ANALYSIS INFORMATION , continued Testing for metals requires acid and heat to pretreat the sample. Since these conditions destroy filter paper, vacuum filtration with glass fiber filter discs is recommended. Also, glass filter discs, unlike paper, do not retain colored species. Temperature Considerations For best results, perform most tests in this manual with sample temperatures between 20 °C (68 °F) and 25 °C (77 °F).
Page 26: Using Pipets And Graduated Cylinders
CHEMICAL ANALYSIS INFORMATION , continued Table 6 Multiplication Factors for Diluting to 100 mL Sample Volume (mL) Multiplication Factor Sample Dilution and Interfering Substances Sample dilution may influence the level at which a substance may interfere. The effect of the interferences decreases as the dilution increases.
Page 27 CHEMICAL ANALYSIS INFORMATION , continued Figure 3 Reading the Meniscus Rinse the pipet or cylinder two or three times with the sample to be tested before filling. Use a pipet filler or pipet bulb to draw the sample into the pipet.
Page 28: Using The Tensette Pipet
For best results use a new tip each time you pipet. After several uses, the pipet tip may retain some liquid, causing inaccurate delivery. Each pipet is supplied with 50 tips; order Hach replacement tips for best results. Always use careful, even hand movements for best reproducibility. If the pipet does not operate smoothly, disassemble and coat the piston and retainer with high-quality stopcock grease.
Page 29: Mixing Water Samples
CHEMICAL ANALYSIS INFORMATION , continued 6. Use the thumb and forefinger to twist the turret cap to the next higher volume position to ensure quantitative transfer of the sample. The “F” position provides full blowout. STEP 6 7. With the tip in contact with the side of the receiving vessel, slowly and smoothly press down on the turret cap until it reaches the stop and the solution is completely discharged.
Page 30 CHEMICAL ANALYSIS INFORMATION , continued Figure 4 Inverting a Sample Cell Figure 5 Swirling a Graduated Cylinder...
Page 31: Using Sample Cells
Using Sample Cells Orientation of Sample Cells Two round sample cells are shipped with the DR/820, DR/850 and DR/890. They are marked with 10-, 20- and 25-mL fill lines which may be used to measure the sample volume unless the procedure instructs you to use other glassware to measure the sample volume.
Page 32: Using Accuvac Ampuls
CHEMICAL ANALYSIS INFORMATION , continued a substantial error in the result. For instance, a 0.1-mL mistake in the dilution of a 1.0-mL final volume produces a 10% error in the test result. Volumes for standard additions can be measured using the 25-mL mark, but it is not recommended for the 10-mL mark due to a potentially excessive relative error.
Page 33: Using Reagent Powder Pillows
CHEMICAL ANALYSIS INFORMATION , continued Using Reagent Powder Pillows Hach uses dry powdered reagents when possible. This minimizes leakage and deterioration problems. Some powders are packaged in individual, pre-measured, polyethylene "powder pillows" or foil pillows called PermaChem pillows. Each pillow contains enough reagent for one test.
Page 34: Reagent And Standard Stability
2. Push 3. Pour Reagent and Standard Stability Hach always strives to make stable formulations and package them to provide maximum protection. Most chemicals and prepared reagents do not deteriorate after manufacture. However, the way they are stored and the packaging can affect how long the reagents are stable. Light, bacterial action, and absorption of moisture and gases from the atmosphere can affect shelf life.
Page 35: Ph Interference
Interference Many of the procedures in this manual only work within a certain pH range. Hach reagents contain buffers to adjust the pH of the typical sample to the correct pH range. However, the reagent buffer may not be strong enough for some samples.
Page 36: Accuracy And Precision
CHEMICAL ANALYSIS INFORMATION , continued Accuracy and Precision Accuracy is the nearness of a test result to the true value. Precision is how closely repeated measurements agree with each other. Although good precision suggests good accuracy, precise results can be inaccurate (see Figure 8).
Page 37 Does the test need a specific sample temperature? f) Is the sample’s pH in the correct range? Hach’s written procedure should help you to answer these questions. 2. Check your reagents. Repeat the Standard Additions using new, fresh reagents. If your results are good, the original reagents were bad.
Page 38 CHEMICAL ANALYSIS INFORMATION , continued Figure 9 Standard Additions Decision Tree Did a Single Standard Addition Give the Correct Recovery? Interferences Interferences Present? Present? Do Multiple Analysis Is Correct Standard Additions On DI Water Give Correct Recovery? Is the Procedure in Do Multiple Standard Use Correct? Additions On Sample...
Page 39 CHEMICAL ANALYSIS INFORMATION , continued The data show several points: • The chemicals, instrument, procedure/technique and standards are working correctly because the iron added to the water sample was completely recovered in the same uniform steps that match the standard addition increments. •...
Page 40 CHEMICAL ANALYSIS INFORMATION , continued time required for the reagent in question. If the reagent(s) is defective, repeat Branch B with new reagents. If the reagents are good, proceed with Branch H. Branch F Examples of non-uniform increments between standard additions are shown below.
Page 41 CHEMICAL ANALYSIS INFORMATION , continued Figure 10 Multiple Standard Additions Graph...
Page 42 CHEMICAL ANALYSIS INFORMATION , continued Branch G Examples of uniform increments between standard additions are given below. Example C mL of Standard Added mg/L Standard Added mg/L Found The plot for sample C illustrates a common interference with a uniform effect on the standard and the substances in the sample.
Page 43: Method Performance
CHEMICAL ANALYSIS INFORMATION , continued Branch H Check operation of the instrument and/or apparatus used to perform the test. Check glassware used in the procedure and make sure it is extremely clean. Dirty pipets and graduated cylinders can cause contamination and will not deliver the correct volume.
Page 44 CHEMICAL ANALYSIS INFORMATION , continued Hach provides a value called the Estimated Detection Limit (EDL) for all programs. It is the calculated lowest average concentration in a deionized water matrix that is different from zero with a 99% level of confidence.
Page 45 CHEMICAL ANALYSIS INFORMATION , continued 5. Compute the MDL using the appropriate Student’s t value (see table below) and the standard deviation value: MDL = Student’s t x s Number of Test Portions Student’s t Value 3.143 2.998 2.896 2.821 For example: The EDL for measuring iron using the FerroZine method is 0.003 mg/L.
Page 46: Precision
CHEMICAL ANALYSIS INFORMATION , continued Note: Occasionally, the calculated MDL may be very different than Hach’s estimate of the detection limit. To test how reasonable the calculated MDL is, repeat the procedure using a standard near the calculated MDL. The average result calculated for the second MDL derivation should agree with the initial calculated MDL.
Page 47: Reagent Blank Correction
Standard Adjust (Adjusting the Standard Curve) The colorimeter has Hach Programs permanently installed in memory. A program usually includes a pre-programmed calibration curve. Each curve is the result of an extensive calibration performed under ideal conditions and is normally adequate for most testing.
Page 48 Adjust the calibration curve using the reading obtained with a Hach Standard Solution or carefully prepared standard made from a concentrated Hach Standard Solution. It is important to adjust the curve in the correct concentration range. For most purposes, Hach recommends adjusting the curve using a standard concentration that is 70 to 85% of the maximum concentration range of the test.
Page 49: Preparing A User-Entered Calibration Curve
CHEMICAL ANALYSIS INFORMATION , continued If you are using a Reagent Blank Correction, the blank correction should be entered before the standard curve is adjusted. To adjust the standard curve: 1. Prepare the standard. 2. Use the standard as the sample in the procedure. 3.
Page 50 CHEMICAL ANALYSIS INFORMATION , continued Figure 11 Logarithmic Calibration Curve mg/L IRON To convert %T readings to concentration, prepare a table such as Table 7 and select the appropriate line from the “%T Tens” column and the appropriate column from the %T Units columns. 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.
Page 51: Usepa Approved And Accepted Definitions
CHEMICAL ANALYSIS INFORMATION , continued Table 7 Calibration Table %T Units Tens 2.30 2.21 2.12 2.04 1.97 1.90 1.83 1.77 1.72 1.66 1.61 1.56 1.51 1.47 1.43 1.39 1.35 1.31 1.27 1.24 1.20 1.17 1.14 1.11 1.08 1.04 1.02 .82. Absorbance Versus Concentration Calibration To read concentration values directly from the instrument, create a user- entered program.
Page 52 USEPA and other regulatory agencies. USEPA Accepted Hach has developed several procedures that are equivalent to USEPA approved methods. Even though minor modifications exist, the USEPA has reviewed and accepted certain procedures for reporting purposes.
Page 53: Section 2 Sample Pretreatment
USEPA presents two digestions (mild and vigorous) for metals analysis. These are much more inconvenient and time consuming compared to the Hach Digesdahl system. Other digestion procedures are required for phosphorus and TKN. EPA Mild Digestion with Hot Plate for Metals Analysis Only 1.
Page 54: Epa Vigorous Digestion With Hot Plate For Metals Analysis Only
SAMPLE PRETREATMENT , continued EPA Vigorous Digestion with Hot Plate for Metals Analysis Only A vigorous digestion can be followed to ensure all organo-metallic bonds are broken. 1. Acidify the entire sample with redistilled 1:1 Nitric Acid Solution to a pH of less than two.
Page 55: General Digesdahl Digestion (Not Usepa Accepted)
Distillation Distillation is an effective way of separating chemical components for analysis. The Hach Distillation Apparatus (see Figure 12) is adapted easily for many test needs and is suitable for water and wastewater samples. Sample distillations are easy and safe to perform.
Page 56 SAMPLE PRETREATMENT , continued Figure 12 General Purpose Distillation Apparatus with Heater and Support Apparatus...
Page 57: Section 3 Waste Management And Safety
SECTION 3 WASTE MANAGEMENT AND SAFETY Waste Management This section provides guidelines for laboratory waste management. It should assist you in complying with USEPA regulations governing waste management. It summarizes basic requirements, but does not contain all USEPA regulations. It does not relieve people from complying with all regulations contained in the Code of Federal Regulations.
Page 58: Hazardous Waste Definition
WASTE MANAGEMENT AND SAFETY , continued The categories are as follows: • Conditionally Exempt Small Quantity Generator - less than 100 kg (220 lb.) per month • Small Quantity Generator - between 100 kg (220 lb.) and 1,000 kg (2,200 lb.) per month •...
Page 59: Characteristic Hazardous Waste Codes
Selected characteristic waste codes for chemicals which may be generated using Hach methods for water analysis are given in the following table. A complete list of waste codes is found in 40 CFR 261.24.
Page 60: Examples Of Hazardous Waste
Examples of Hazardous Waste A number of chemicals used in and final solutions created from Hach procedures are hazardous wastes when they are disposed. In addition, substances in the sample matrix may be a hazardous waste. Sometimes, reagents which would be hazardous are neutralized or changed during the analytical procedure.
Page 61: Management Of Specific Wastes
Pages under “Waste Disposal - 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 obtain the following documents by calling 1-800-227-4224 or 970-669-3050 and requesting the literature...
Page 62: Resources
WASTE MANAGEMENT AND SAFETY , continued If a cyanide-containing compound is spilled, you must be careful not to be exposed to hydrogen cyanide gas. Take the following steps to destroy the cyanide compounds in an emergency: a) Use a fume hood, supplied air or self-contained breathing apparatus. b) While stirring, add the waste to a beaker containing a strong solution of sodium hydroxide and either calcium hypochlorite or sodium hypochlorite (household bleach).
Page 63: Material Safety Data Sheets
MSDS and how to locate important information for safety and waste disposal. The information provided on the MSDS applies to the product as sold by Hach. The properties of any mixtures obtained by using this product will be different. How to Obtain an MSDS Hach ships an MSDS to each customer with the first order of any chemical product.
Page 64 WASTE MANAGEMENT AND SAFETY , continued 1 Product Identification This section contains: • Hach product name • Chemical Abstract Services (CAS) number • Chemical name • Chemical formula, if appropriate • Chemical family to which the material belongs 2 Ingredients This section lists each component in the product.
Page 65 WASTE MANAGEMENT AND SAFETY , continued 4 Fire, Explosion Hazard And Reactivity Data This section contains the flash point and flammable limits of the material. It also includes how to fight fires if the material catches on fire. Key terms in this section include: •...
Page 66: Safety
WASTE MANAGEMENT AND SAFETY , continued 9 Transportation Data Domestic and International shipping information is provided in this section. It gives shipping name, hazard class, and ID number of the product. 10 References This section lists the reference materials used to write the MSDS. Following the Reference section, the product is listed as having SARA 313 chemicals or California Proposition 65 List Chemicals, if applicable.
Page 67: First Aid Equipment And Supplies
WASTE MANAGEMENT AND SAFETY , continued • Laboratory coats or splash aprons to protect skin and clothing from splashes. • Footwear to protect feet from spills. Open toed shoes should not be worn in chemistry settings. • Respirators may be needed to protect you from breathing toxic vapors if adequate ventilation, such as fume hoods, are not available.
Page 68: Osha Chemical Hygiene Plan
WASTE MANAGEMENT AND SAFETY , continued 9. Do not block exits or emergency equipment. OSHA Chemical Hygiene Plan The Occupational Safety and Health 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 chemicals.
Page 69: Section 4 Procedures
SECTION 4 PROCEDURES...
Page 71: Aluminum Aluminon Method
Method 8012 ALUMINUM (0 to 0.80 mg/L) For water and wastewater Aluminon Method Enter the stored Press: Fill a 50-mL Add the contents of 1 ENTER program number for graduated mixing one Ascorbic Acid The display will show aluminum (Al). cylinder to the 50-mL Powder Pillow.
Page 72 ALUMINUM, continued The display will Pour the 25 mL of The display will Within three show: 00:30 Timer 2 mixture in the cylinder show: 15:00 TIMER 3 minutes after the timer into a second 25-mL beeps, place the blank Press: Press: ENTER ENTER...
Page 73 ALUMINUM, continued Sampling and Storage Collect samples in a clean glass or plastic container. Preserve the sample by adjusting the pH to 2 or less with nitric acid (about 1.5 mL per liter). Preserved samples can be stored up to six months at room temperature. Before analysis, adjust the pH to 3.5–4.5 with 5.0 N Sodium Hydroxide.
Page 74 ALUMINUM, continued Estimated Detection Limit The estimated detection limit for program #1 is 0.013 mg/L Al. For more information on the estimated detection limit, see Section 1. Interferences Interfering Interference Levels and Treatments Substance Acidity Acidity interferes at greater than 300 mg/L as CaCO .
Page 75 ALUMINUM, continued 1. Select the vertical grid line along the top of the graph that represents the aluminum reading obtained in Step 15. 2. Locate the point of the vertical line (instrument reading) where it intersects with the horizontal grid line that indicates how much fluoride is present in the sample.
Page 76 Pipet Tips, for 19700-01 TenSette Pipet ..........1000/pkg..21856-28 Pipet, Volumetric, Class A, 1.00 mL ............each..14515-35 Thermometer, –20 to 110 °C, non-mercury ..........each..26357-02 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 77: Bromine, Dpd Method
Method 8016 BROMINE (0 to 4.50 mg/L) For water, wastewater, and seawater DPD Method (Powder Pillows or AccuVac Ampuls) Using Powder Pillows Enter the stored Press: Fill a sample cell Place the blank into 5 ENTER program number for with 10 mL of sample the cell holder.
Page 78 BROMINE, continued 5. Press: Add the contents of Press: When the timer ZERO TIMER one DPD Total Chlorine beeps, place the sample ENTER The cursor will move to Powder Pillow to the into the cell holder. the right, then the A three-minute reaction sample cell (the Tightly cover the sample...
Page 79 BROMINE, continued Using AccuVac Ampuls Enter the stored Press: Fill a sample cell Place the blank in the 6 ENTER program number for with at least 10 mL of cell holder. Tightly The display will show bromine (Br sample (the blank). cover the sample cell mg/L, Br2 and the AccuVac Ampuls.
Page 80 BROMINE, continued After the timer beeps, Press: READ place the AccuVac The cursor will move to ampul into the cell the right, then the result holder. Tightly cover the in mg/L bromine will ampule with the be displayed. instrument cap. Note: If the sample Note: Standard Adjust may temporarily turns yellow...
Page 81 BROMINE, continued Perform the bromine analysis immediately after collection. 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 the reacted sample (this is the spiked sample).
Page 82 ± 0.02 mg/L bromine. Estimated Detection Limit The estimated detection limit for program 5 is 0.04 mg/L Br 0.03 mg/L Br for program 6. For more information on derivation and use of Hach’s estimated detection limit, see Section 1.
Page 83 BROMINE, continued Interferences Interfering Substance Interference Level and Treatment Acidity Greater than 150 mg/L CaCO . May not develop full color or color may fade instantly. Neutralize to pH 6-7 with 1 N sodium hydroxide. Determine amount to be added on separate sample aliquot, then add the same amount to the sample being tested.
Page 84 Pipet Tips, for 19700-01 TenSette Pipet ..........50/pkg..21856-96 Pipet Tips, for 19700-01 TenSette Pipet ..........1000/pkg..21856-28 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you. * Contact Hach for larger sizes...
Page 85 CHLORAMINE, MONO, Low Range (0–4.50 mg/L Cl Method 10171 Indophenol Method For chlorinated drinking water and chlorinated wastewater Slot Enter the user Press: Fill the 10-mL/1-cm Place the cell into program number for cell to the 10-mL line the instrument. Tightly 110 ENTER monochloramine.
Page 86 CHLORAMINE, MONO, Low Range, continued Press: READ The cursor will move to the right, then the result in mg/L monochloramine (as Cl or chosen units) will be displayed. Sampling and Storage Analyze samples for monochloramine immediately after collection. If sampling with the sample cell, rinse the sample cell several times with the sample, then carefully fill to the 10-mL mark.
Page 87 CHLORAMINE, MONO, Low Range, continued 6. Obtain a recent lot of Chlorine Solution Ampules, 50–70 mg/L, and note the actual free chlorine concentration for this lot. 7. Calculate the amount of Chlorine Solution to be added to the ammonia standard using the following equation: mL chlorine solution required --------------------------------------------------------------- - free chlorine concentration...
Page 88 CHLORAMINE, MONO, Low Range, continued Table 9 Non-interfering Substances (Continued) Substance Maximum Level Tested Bromine 15 mg/L Br Calcium 1000 mg/L CaCO Chloride 18,000 mg/L Chlorine Dioxide 5 mg/L ClO Chromium (III) 5 mg/L Copper 10 mg/L Cyanide 10 mg/L CN Free chlorine 10 mg/L Cl Glycine...
Page 89 Minutes ° C ° F >25 >77 Instrument Setup This procedure will add the current method as a new Hach program to your DR/850 or DR/890. 1. Turn on the instrument by pressing the key. 2. Press the key. SETUP 3.
Page 90 CHLORAMINE, MONO, Low Range, continued Line Number Entry Line Number Entry...
Page 91 CHLORAMINE, MONO, Low Range, continued REQUIRED REAGENTS Quantity Required Description Per Test Unit Cat. No. Monochlor F Reagent Pillows..........1..50/pkg....28022-46 REQUIRED APPARATUS Sample Cell, 10-mL/1-cm ............1..2/pkg....48643-02 Clippers, shears ..............1...each....23694-00 OPTIONAL REAGENTS Rochelle Salt Solution ...............29-mL DB....1725-33 Organic-Free Water ................
Page 93: Method
CHLORAMINE, MONO, High Range (0–10.0 mg/L Cl Method 10172 Indophenol Method For chlorinated drinking water and chlorinated wastewater Enter the user Press: Insert the COD/TNT Remove the cap program number for Vial Adapter into the from one HR 111 ENTER Chloramine, HR.
Page 94 CHLORAMINE, MONO, High Range, continued After the timer Press: READ. beeps, wipe the prepared The cursor will move to vial and place it into the the right , then the instrument. Cover the results in mg/L sample vial tightly with monochloramine (as the instrument cap.
Page 95 CHLORAMINE, MONO, High Range, continued 6. Calculate the amount of Chlorine Solution to be added to the ammonia standard using the following equation: mL chlorine solution required --------------------------------------------------------------- - free chlorine concentration 7. Turn the stir plate on to medium speed. 8.
Page 96 CHLORAMINE, MONO, High Range, continued Table 11 Non-interfering Substances (Continued) Substance Maximum Level Tested Chloride 18,000 mg/L Chlorine Dioxide 5 mg/L ClO Chromium (III) 5 mg/L Copper 10 mg/L – Cyanide 10 mg/L CN Free Chlorine 10 mg/L Cl Glycine 1 mg/L N Iron (II) 10 mg/L...
Page 97 Consult the Material 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 instrument on by pressing the key.
Page 98 CHLORAMINE, MONO, High Range, continued Table 13 (Continued)
Page 99 CHLORAMINE, MONO, High Range, continued REQUIRED REAGENTS Quantity Required Description Per Test Unit Cat. No. HR Monochloramine Test ‘N Tubes, 50 tests ........28051-45 Includes: ........* HR Monochloramine Diluent Vials ..........50 Funnel, micro..............1...each....25843-35 Monochlor F Reagent Pillows ......... 1..50/pkg....28022-46 REQUIRED APPARATUS COD/TNT Vial Adapter, DR/800 ..........
Page 101: Chlorine, Free, Ultra-High Range, Dpd Method
CHLORINE, FREE, Ultra-high Range (0.0–10.0 mg/L Cl Method 10069 DPD Method USEPA accepted for reporting drinking water analyses For testing higher levels of free chlorine (hypochlorous acid and hypochlorite) in drinking water, cooling water, and industrial process waters Note: This product has not been evaluated to test for chlorine and chloramines in medical applications in the United States.
Page 102 CHLORINE, FREE, Ultra-high Range, continued Slot Press: Remove the sample Place the sample cell Within one minute ZERO cell from the cell holder into the instrument. after reagent addition, The cursor will move to and add the contents of Cover the sample cell press: READ the right, then the...
Page 103 CHLORINE, FREE, Ultra-high Range, continued • A common error in testing for chlorine is failure to obtain a representative sample. If sampling from a tap, let the water flow for at least five minutes to ensure a representative sample. Let the sample container overflow with sample several times.
Page 104 CHLORINE, FREE, Ultra-high Range, continued Method Performance Precision In a single laboratory, using a chlorine standard solution of 5.05 mg/L Cl and representative lots of reagent, a single operator obtained a standard deviation of ± 0.05 mg/L Cl Estimated Detection Limit The estimated detection limit for Method 10069 is 0.1 mg/L Cl For more information on the estimated detection limit, see Section 1 of the DR/800 Procedure Manual.
Page 105 DPD (N,N-diethyl-p-phenylenediamine) indicator to form a pink color which is proportional in intensity to the chlorine concentration. Instrument Setup The following procedure will add this method as a new Hach program to a DR/800 instrument. 1. Turn on the instrument by pressing the key.
Page 106 CHLORINE, FREE, Ultra-high Range, continued 6. Key the number in the “Enter” column corresponding to line number 1 on the display. Press . Repeat for lines 2–56 ENTER on the display. Line Number Enter Line Number Enter...
Page 107 CHLORINE, FREE, Ultra-high Range, continued REQUIRED REAGENTS Quantity Required Description Per Test Unit Cat. No. DPD Free Chlorine Reagent Powder Pillows, 25-mL.... 1..100/pkg....14070-99 REQUIRED APPARATUS Sample Cell, 10-mL/1-cm ............1..2/pkg....48643-02 OPTIONAL REAGENTS ® Chlorine Standard Solution, 2-mL Voluette Ampule, 50–75 mg/L................
Page 109: Chlorine, Total, Ultra-High Range, Dpd Method
CHLORINE, TOTAL, Ultra-High Range (0.0–10.0 mg/L Cl ) Method 10070 DPD Method USEPA accepted for reporting water and wastewater analyses For testing higher levels of total chlorine (free and combined) in drinking water, cooling water, industrial process waters, or treated wastewater Note: This product has not been evaluated to test for chlorine and chloramines in medical applications in the United States.
Page 110 CHLORINE, TOTAL, Ultra-High Range, continued Slot Press: Remove the sample Press: Within 3 minutes ZERO cell from the cell holder after the timer beeps, TIMER ENTER The cursor will move to and add the contents of place the sample cell the right, then the A 3-minute reaction one 25- mL DPD Total...
Page 111 CHLORINE, TOTAL, Ultra-High Range, continued Sampling and Storage Analyze samples for chlorine immediately after collection. Free and combined chlorine are strong oxidizing agents and react rapidly with various compounds. Many factors such as sunlight, pH, temperature, and sample composition will influence decomposition of chlorine in water.
Page 112 CHLORINE, TOTAL, Ultra-High Range, continued 4. Calculate the concentration of mg/L chlorine added to each sample. × volume of standard added label value of Cl standard ampule mg/L chlorine added ------------------------------------------------------------------------------------------------------------------------------------------------------ - sample volume volume of standard added The spiked sample results should reflect the analyzed sample result plus the calculated mg/L Cl added to each sample.
Page 113 Instrument Setup The following procedure will add this method as a new Hach program to a DR/800 instrument. 1. Turn on the instrument by pressing the key.
Page 114 CHLORINE, TOTAL, Ultra-High Range, continued Line Number Enter Line Number Enter...
Page 115 CHLORINE, TOTAL, Ultra-High Range, continued REQUIRED REAGENTS Quantity Required Description Per Test Unit Cat. No. DPD Total Chlorine Reagent Powder Pillows, 25-mL ..1..100/pkg....14064-99 REQUIRED APPARATUS Sample Cell, 10-mL/1-cm ............1..2/pkg....48643-02 OPTIONAL REAGENTS ® Chlorine Standard Solution, 2-mL Voluette Ampule, 50–75 mg/L................
Page 117: Chlorine, Free, Dpd Method
Method 8021 CHLORINE, FREE (0 to 2.00 mg/L) For water, wastewater, and seawater DPD Method (Powder Pillows or AccuVac Ampuls)USEPA accepted for reporting wastewater and drinking water analyses Note: This product has not been evaluated to test for chlorine and chloramines in medical applications in the United States.
Page 118 CHLORINE, FREE, continued 5. Press: Fill another cell with Add the contents of Immediately place ZERO 10 mL of sample. one DPD Free Chlorine the prepared sample into The cursor will move to Powder Pillow to the the cell holder. Tightly the right, then the sample cell (the cover the sample cell...
Page 119 CHLORINE, FREE continued Using AccuVac Ampuls Enter the stored Press: Fill a sample cell Place the blank into 11 ENTER program number for free with at least 10 mL of the cell holder. Tightly The display will show and total chlorine (Cl sample (the blank).
Page 120 CHLORINE, FREE continued Press: Note: If the sample READ temporarily turns yellow The cursor will move to after reagent addition, or the right, then the result the display flashes “limit”, in mg/L chlorine will it is due to high chlorine be displayed.
Page 121 CHLORINE, FREE continued A common error in testing for chlorine 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 sample. Let the container overflow with the sample several times, then cap the sample container so there is no headspace (air) above the sample.
Page 122 ±0.01 mg/L chlorine. Estimated Detection Limit (EDL) The estimated detection limit for programs 9 and 11 is 0.02 mg/L . For more information on derivation and use of Hach’s estimated detection limit, see Section 1. Pollution Prevention and Waste Management...
Page 123 CHLORINE, FREE continued Interferences Interfering Substance Interference Level and Treatment Acidity Greater than 150 mg/L CaCO . May not develop full color or color may fade instantly. Neutralize to pH 6-7 with 1 N sodium hydroxide. Determine amount to be added on separate sample aliquot, then add the same amount to the sample being tested.
Page 124 Tips, for 19700-01 TenSette Pipet ............. 1000/pkg..21856-28 PourRite Ampule Breaker................each..24846-00 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you. * Marked Dropper Bottle - contact Hach for larger sizes.
Page 125: Chlorine, Total Dpd Method
Method 8167 CHLORINE, TOTAL (0 to 2.00 mg/L) For water, wastewater and seawater DPD Method (Powder Pillows or AccuVac Ampuls) USEPA accepted for reporting water and wastewater analyses Note: This product has not been evaluated to test for chlorine and chloramines in medical applications in the United States.
Page 126 CHLORINE, TOTAL, continued Press Fill a second cell to Add the contents of Press: ZERO the 10-mL mark with one DPD Total Chlorine The cursor will move to TIMER ENTER sample. Powder Pillow to the the right, then the A three-minute reaction sample cell (the display will show: period will begin.
Page 127 CHLORINE, TOTAL, continued Using AccuVac Ampuls Enter the stored Press: Fill a sample cell Place the blank into 11 ENTER program number for with at least 10 mL of the cell holder. Tightly The display will show total chlorine (Cl sample (the blank).
Page 128 CHLORINE, TOTAL, continued When the timer Press: READ beeps, place the The cursor will move to AccuVac Ampul into the the right, then the result cell holder. Tightly in mg/L total chlorine cover the ampule with will be displayed. the instrument cap. Note: If the sample Note: Standard Adjust may temporarily turns yellow...
Page 129 CHLORINE, TOTAL, continued Do not use the same sample cells for free and total chlorine. If trace iodide from the total chlorine reagent is carried over into the free chlorine determination, monochloramine will interfere. It is best to use separate, dedicated sample cells for free and total chlorine determinations.
Page 130 ±0.01 mg/L chlorine. Estimated Detection Limit (EDL) The estimated detection limit for programs 9 and 11 is 0.02 mg/L . For more information on derivation and use of Hach’s estimated detection limit, see Section 1.
Page 131 CHLORINE, TOTAL, continued Interferences Interfering Substance Interference Level and Treatment Acidity Greater than 150 mg/L CaCO . May not develop full color or color may fade instantly. Neutralize to pH 6-7 with 1 N sodium hydroxide. Determine amount to be added on separate sample aliquot, then add the same amount to the sample being tested.
Page 132 Pipet Tips, for 19700-01 TenSette Pipet ..........50/pkg..21856-96 Pipet Tips, for 19700-01 TenSette Pipet ..........1000/pkg..21856-28 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you. * Marked Dropper Bottle - contact Hach for larger sizes.
Page 133: Chlorine, Free, Dpd Test 'N Tube™ Method
Cl2 and the chlorine (Cl adapter until it drops ZERO icon. Note: Fill to the top of the into place. Then push Hach logo “oval” mark. Press: PRGM down fully to insert it. Note: Samples must be The display will show:...
Page 134 READ it in the adapter. Note: Fill to the top of the Note: Use slow, deliberate The cursor will move to Hach logo “oval” mark. inversion for complete Push straight down on the right, then the result recovery. Ten inversions...
Page 135 CHLORINE, FREE continued Sampling and Storage Analyze samples for chlorine immediately after collection. Free chlorine is a strong oxidizing agent and is unstable in natural waters. It reacts rapidly with various inorganic compounds and more slowly oxidizes organic compounds. Many factors, including reactant concentrations, sunlight, pH, temperature, and salinity influence decomposition of free chlorine in water.
Page 136 ±0.14 mg/L chlorine. Estimated Detection Limit (EDL) The estimated detection limit for program 10 is 0.03 mg/L Cl For more information on derivation and use of Hach’s estimated detection limit, see Section 1. Interferences Interfering Substance...
Page 137 CHLORINE, FREE continued Interfering Substance Interference Level and Treatment Monochloramine For conventional free 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 sample temperature, relative amount of monochloramine to free chlorine, and the time required to do the analysis.
Page 138 Pipet, TenSette, 0.1 to 1.0 mL ..............each ..19700-01 Pipet Tips, for 19700-01 TenSette Pipet ..........50/pkg..21856-96 Pipet Tips, for 19700-01 TenSette Pipet ..........1000/pkg..21856-28 PourRite Ampule Breaker................each..24846-00 Test Tube Rack ................... each..18641-00 * Marked Dropper Bottle - contact Hach for larger sizes.
Page 141: Chlorine, Total, Dpd Test 'N Tube™ Method
Cl2 and the chlorine (Cl the adapter until it drops ZERO icon. Note: Fill to the top of the into place. Then push Hach logo “oval” mark. Press: PRGM down to fully insert it. Note: Samples must be The display will show:...
Page 142 Note: Fill to the top of the the right, then the removes fingerprints and Hach logo “oval” mark. adapter. display will show: other marks. Note: A pink color will Note: Do not move the vial 0.00 mg/L Cl2...
Page 143 CHLORINE, TOTAL, continued Sampling and Storage Analyze samples for chlorine immediately after collection. Free and combined chlorine are strong oxidizing agents and are unstable in natural waters. They react rapidly with various inorganic compounds and more slowly oxidizes organic compounds. Many factors, including reactant concentrations, sunlight, pH, temperature and salinity influence decomposition of chlorine in water.
Page 144 ±0.14 mg/L chlorine. Estimated Detection Limit (EDL) The estimated detection limit for programs 10 is 0.03 mg/L Cl For more information on derivation and use of Hach’s estimated detection limit, see Section 1. Interferences Interfering...
Page 145 CHLORINE, TOTAL, continued Summary of Method Chlorine can be present in water as free available chlorine and as combined available chlorine. Both forms can exist in the same water and be determined together as the total available chlorine. Free chlorine is present as hypochlorous acid and/or hypochlorite ion.
Page 146 Pipet, TenSette, 0.1 to 1.0 mL..............each..19700-01 Pipet Tips, for 19700-01 TenSette Pipet ..........50/pkg..21856-96 Pipet Tips, for 19700-01 TenSette Pipet ..........1000/pkg..21856-28 Test Tube Rack ................... each..18641-00 * Marked Dropper Bottle - contact Hach for larger sizes.
Page 147: Chlorine Dioxide, Dpd Method
CHLORINE DIOXIDE (0 to 5.00 mg/L) Method 10126 DPD Method For water USEPA accepted for reporting for drinking water analysis Note: This product has not been evaluated to test for chlorine and chloramines in medical applications in the United States. Using Powder Pillows Enter the stored Press:...
Page 148 CHLORINE DIOXIDE, continued Press: Add four drops of Add the contents of Allow 30 seconds ZERO Glycine Reagent to the one DPD Free Chlorine for undissolved powder The cursor will move to sample cell. Swirl to Powder Pillow to the to settle.
Page 149 CHLORINE DIOXIDE, continued ® Using AccuVac Ampuls Enter the stored Press: Fill a sample cell Place the blank into 113 ENTER program number for with at least 10 mL of the cell holder. Tightly The display will show chlorine dioxide (ClO sample (the blank).
Page 150 CHLORINE DIOXIDE, continued Note: If the sample temporarily turns yellow Allow 30 seconds Press: READ after reagent addition, or the for undissolved powder The cursor will move to display flashes “limit”, it is to settle. Place the due to high chlorine dioxide the right, then the result AccuVac Ampul into the levels.
Page 151 Dilute 1 drop of commercial 5% chlorine bleach in 1 liter of chlorine demand-free deionized water. Use this as the standard. 2. Verify the standard’s concentration using the Hach Free Chlorine Method, #8021. 3. Perform the chlorine dioxide test on the standard without adding glycine (step 6).
Page 152 Program 0.04 mg/L ClO 0.04 mg/L ClO For more information on derivation and use of Hach’s estimated detection limit, see Section 1 of the DR/800 Procedures Manual. Interferences A substance interferes if it changes the final reading by 0.1 mg/L or more.
Page 153 CHLORINE DIOXIDE, continued Interfering Substance Interference Levels and Treatments Iodine, I Interferes at all levels. Manganese, oxidized Oxidized manganese interferes at all levels. Oxidized chromium interferes at levels , Mn greater than 2 mg/L. To remove the interferences: Adjust sample pH to 6 –7. Chromium, oxidized Add 3 drops potassium iodide (30 g/L) to a 25-mL sample.
Page 154 Pipet ........1000/pkg ....21856-28 ™ PourRite Ampule Breaker ..............each ....24846-00 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you. * Marked Dropper Bottle - contact Hach for larger sizes.
Page 155: Cyanide, Pyridine-Pyrazalone Method
Method 8027 CYANIDE (0 to 0.240 mg/L) For water, wastewater, and seawater Pyridine-Pyrazalone Method Enter the stored Press: Fill a sample cell Add the contents of 23 ENTER program number for with 10-mL of sample. one CyaniVer 3 Cyanide The display will show cyanide (CN).
Page 156 CYANIDE, continued :10 seconds :30 seconds Press: After the first timer After the timer beeps, Shake the sample cell TIMER beeps, the display will add the contents of one for ten seconds. ENTER show: 0:30 TIMER 2 CyaniVer 4 Cyanide Immediately proceed A 30-second reaction Reagent Powder Pillow.
Page 157 CYANIDE, continued Place the blank into Press: Place the prepared Press: ZERO READ the cell holder. Tightly sample into the cell The cursor will move to The cursor will move to cover the sample cell holder. Tightly cover the the right, then the the right, then the result with the instrument cap.
Page 158 CYANIDE, continued Solution. If significant amounts of preservative are used, correct for the volume added; see Correction for Volume Additions in Section 1 for more information. Oxidizing Agents Oxidizing agents such as chlorine decompose cyanides during storage. To test for their presence and eliminate their effect, pretreat the sample as follows: a) Take a 25-mL portion of the sample and add one drop of...
Page 159 CYANIDE, continued b) If the test paper darkens, add a 1-g measuring spoon of lead acetate to the sample. Repeat Step a. (Purchase lead acetate from a local supplier.) c) If the test paper continues to turn dark, keep adding lead acetate until the sample tests negative for sulfide.
Page 160 CYANIDE, continued Immediately before use, prepare a 0.10 mg/L cyanide working solution by diluting 1.00 mL of the 100 mg/L stock solution to 1000 mL using deionized water. Use this prepared standard in place of sample in Step 3. Results should be 0.10 mg/L CN –...
Page 161 CYANIDE, continued c) Add Sodium Arsenite Solution drop-wise until the sample turns colorless. Swirl the sample thoroughly after each drop. Count the number of drops. d) Take another 25-mL sample and add the total number of drops of Hydrochloric Acid Standard Solution counted in Step a.
Page 162 CYANIDE, continued Acid Distillation For USEPA reporting purposes, samples must be distilled. All samples should be treated by acid distillation except when experience has shown that there is no difference in results obtained with or without distillation. With most compounds, a one-hour reflux is adequate.
Page 163 Distillation Procedures A detailed procedure for the distillation of cyanide samples is included with the Hach Distillation Apparatus. Three detailed procedures, Free Cyanides, Cyanides Amenable to Chlorination, and Total Cyanides, are included with the four- and ten-position Midi-Dist Distillation System. See the Optional Apparatus listing.
Page 164 Support Ring, 4 inch ................... each..... 580-01 Support Stand....................each....563-00 Thermometer, –20 to 110 °C, non-mercury ..........each..26357-02 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 165: Cyanuric Acid Turbidimetric Method
Method 8139 CYANURIC ACID (7 to 55 mg/L) For water, pools and spas Turbidimetric Method Enter the stored Press: Fill a sample cell Place the blank into 24 ENTER program number for with 25 mL of sample the cell holder. Tightly The display will show cyanuric acid.
Page 166 CYANURIC ACID, continued Place the prepared Press: READ sample into the cell The cursor will move to holder. Tightly cover the right, then the result the sample cell with the in mg/L cyanuric acid instrument cap. will be displayed. Note: Standard Adjust may be performed using a prepared standard (see Section 1).
Page 167 Flask, volumetric, Class A, 1000 mL............each ..14574-53 Funnel, poly, 65 mm..................each ... 1083-67 Pipet, Bulb....................each ..14651-00 Pipet, volumetric, Class A, 2.00 mL ............each ..14515-36 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 169: Fluoride, Spadns Method
Method 8029 FLUORIDE (0 to 2.00 mg/L F For water, wastewater and seawater SPADNS Method (Reagent Solution or AccuVac Ampuls) Using SPADNS Reagent Solution Enter the stored Press: Pipet 10.0 mL of Measure 10.0 mL of 27 ENTER program number for sample into a dry 10-mL deionized water into a The display will show...
Page 170 FLUORIDE, continued Place the prepared Press: READ sample into the cell The cursor will move to holder. Tightly cover the the right, then the result sample cell with the in mg/L fluoride will be instrument cap. displayed. Note: Use of the Standard Adjust feature with each new lot of reagent is highly recommended.
Page 171 FLUORIDE, continued Quickly invert the Press: After the timer beeps Press: ZERO ampules several times to place the blank into the TIMER ENTER The cursor will move to mix. Wipe off any cell holder. Tightly the right, then the A one-minute reaction liquid or fingerprints.
Page 172 Accuracy Check Standard Solution Method A variety of standard solutions covering the entire range of the test are available from Hach. Use these in place of sample to verify technique. Minor variations between lots of reagent become measurable above 1.5 mg/L. While results in this region are usable for most purposes, better accuracy may be obtained by diluting a fresh sample 1:1 with deionized water and retesting.
Page 173 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. See the Hach Distillation Apparatus Manual. Turn on the water and make certain it is flowing through the condenser.
Page 174 FLUORIDE, continued d) Turn the heat control to setting 10, with the thermometer in place. The yellow pilot lamp shows when the heater is e) When the temperature reaches 180 °C (about one hour), turn the still off. f) Dilute the collected distillate to 100 mL, if necessary. Analyze the distillate by the above method.
Page 175 1, portable, with electrode...........each ..51700-10 Pipet, TenSette, 1.0 to 10.0 mL ..............each ..19700-10 Pipet Tips, for 19700-10 TenSette Pipet ..........50/pkg ..21997-96 Stopper ......................6/pkg ....1731-06 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 177: Fluoride, Spadns 2 Method
* Adapted from Standard Methods for the Examination of Water and Wastewater. Per USEPA Rules and Regulations at 40 CFR 136.6, Method Modifications and Analytical Requirements, Hach Method 10225 (SPADNS 2) for the determination of fluoride in water is equivalent to the EPA Reference Method SM 4500-F D.
Page 178 FLUORIDE, continued Place the prepared Press: READ sample into the cell The cursor will move to holder. Tightly cover the the right, then the result sample cell with the in mg/L fluoride will be instrument cap. displayed. Note: Use of the Standard Adjust feature with each new lot of reagent is highly recommended.
Page 179 FLUORIDE, continued Cap and quickly Press: After the timer beeps Press: ZERO invert the ampules place the blank into the TIMER ENTER The cursor will move to several times to mix. cell holder. Tightly the right, then the A one-minute reaction Wipe off any liquid or cover the ampule with display will show:...
Page 180 Accuracy Check Standard Solution Method A variety of standard solutions covering the entire range of the test are available from Hach. Use these in place of sample to verify technique. Minor variations between lots of reagent become measurable above 1.5 mg/L. While results in this region are usable for most purposes, better accuracy may be obtained by diluting a fresh sample 1:1 with deionized water and retesting.
Page 181 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. See the Hach Distillation Apparatus Manual. Turn on the water and make certain it is flowing through the condenser.
Page 182 FLUORIDE, continued mg/L chloride present. d) Turn the heat control to setting 10, with the thermometer in place. The yellow pilot lamp shows when the heater is e) When the temperature reaches 180 °C (about one hour), turn the still off. f) Dilute the collected distillate to 100 mL, if necessary.
Page 183 1, portable, with electrode...........each ..51700-10 Pipet, TenSette, 1.0 to 10.0 mL ..............each ..19700-10 Pipet Tips, for 19700-10 TenSette Pipet ..........50/pkg ..21997-96 Stopper ......................6/pkg ....1731-06 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 185: Hardness, Calcium And Magnesium; Calmagite Colorimetric Method
Method 8030 HARDNESS (0 to 4.00 mg/L Ca and Mg as CaCO ) For water, wastewater, seawater Calcium and Magnesium; Calmagite Colorimetric Method Enter the stored Press: Pour 100 mL of Add 1.0 mL of 30 ENTER program number for sample into a 100-mL Calcium and The display will show...
Page 186 HARDNESS, continued Place the blank into Press: Place the prepared Press: ZERO READ the cell holder. Tightly sample into the cell The cursor will move to The cursor will move to cover the sample cell with holder. Tightly cover the the right, then the the right, then the result the instrument cap.
Page 187 HARDNESS, continued between 3 and 8 with 5.0 N Sodium Hydroxide Standard Solution just before analysis. Correct the test results for volume additions; see Correction for Volume Additions in Section 1 for more information. Accuracy Check Using a 2.00 mg/L (as CaCO ) standard solution as sample, perform the hardness procedure described above.
Page 188 HARDNESS, continued Summary of Method The colorimetric method for measuring hardness supplements the conventional titrimetric method because it can measure very low levels of calcium and magnesium. Also some interfering metals (those listed above) in the titrimetric method are inconsequential in the colorimetric method when diluting the sample to bring it within the range of this test.
Page 189: Iron, Ferrous, 1,10 Phenanthroline Method
Method 8146 IRON, FERROUS (0 to 3.00 mg/L) For water, wastewater, and seawater 1,10 Phenanthroline Method (Powder Pillows or AccuVac Ampuls) Using Powder Pillows Enter the stored Press: Fill a sample cell Place the blank into 33 ENTER program number for with 25 mL of sample the cell holder.
Page 190 IRON, FERROUS, continued Place the prepared Press: READ sample into the cell The cursor will move to holder. Tightly cover the the right, then the result sample cell with the in mg/L ferrous iron will instrument cap. be displayed. Note: Standard Adjust may be performed using a prepared standard (see Section 1).
Page 191 IRON, FERROUS, continued Press: Fill a Ferrous Quickly invert the Press: ZERO Iron AccuVac Ampul ampul several times to The cursor will move to TIMER ENTER with sample. mix. Wipe off any liquid the right, then the A three-minute reaction or fingerprints.
Page 192 IRON, FERROUS, continued Sampling and Storage Ferrous iron must be analyzed immediately and cannot be stored. Analyze samples as soon as possible to prevent oxidation of ferrous iron to ferric iron, which is not measured. Accuracy Check Standard Solution Method Prepare a ferrous iron stock solution (100 mg/L Fe ) by dissolving 0.7022 grams of ferrous ammonium sulfate,...
Page 193 Pipet, volumetric, Class A, 1.00 mL ............each ..14515-35 Pipet Filler, safety bulb ................each ..14651-00 Weighing Boat, 67/46 mm, 8.9 cm square ..........500/pkg ..21790-00 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 195: Iron, Total, Ferrover Method
Method 8008 IRON, TOTAL (0 to 3.00 mg/L) For water, wastewater, and seawater FerroVer Method (Powder Pillows or AccuVac Ampuls) USEPA approved for reporting wastewater analysis (digestion is required; see Section 2 Enter the stored Press: Fill a clean sample Place the blank into 33 ENTER program number for iron...
Page 196 IRON, TOTAL, continued Place the prepared Press: READ sample into the cell The cursor will move to holder. Tightly cover the the right, then the result sample cell with the in mg/L iron (Fe) will instrument cap. be displayed. Note: Standard Adjust may be performed using a prepared standard (see Section 1).
Page 197 IRON, TOTAL, continued Press: Fill a FerroVer Quickly invert the Press: ZERO AccuVac Ampul ampul several times to The cursor will move to TIMER ENTER with sample. mix. Wipe off any liquid the right, then the A three-minute reaction or fingerprints. display will show: Note: Keep the tip period will begin.
Page 198 IRON, TOTAL, continued Sampling and Storage Collect samples in acid-cleaned glass or plastic containers. No acid addition is necessary if analyzing the sample immediately. To preserve samples, adjust the pH to 2 or less with nitric acid (about 2 mL per liter). Preserved samples may be stored up to six months at room temperature.
Page 199 ±0.009 mg/L Fe. Estimated Detection Limit (EDL) The EDL for program 33 is 0.03 mg/L Fe. For more information on derivation and use of Hach’s estimated detection limit, see Section 1. Interferences Interfering Substances and Suggested Treatments...
Page 200 IRON, TOTAL, continued Interfering Substance Interference Level and Treatment Turbidity 1. Add 0.1 g scoop of RoVer Rust Remover to the blank in Step 3. Swirl to mix. 2. Zero the instrument with this blank. 3. If sample remains turbid, add three 0.2 g scoops of RoVer to a 75-mL sample.
Page 201 Pipet Tips, for 19700-01 TenSette Pipet ..........1000/pkg ..21856-28 Pipet, volumetric, Class A, 1.00 mL ............each ..14515-35 Spoon, measuring, 0.1 g ................each ....511-00 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 203: Iron, Total, Ferromo ™ Method
Method 8365 IRON, TOTAL (0 to 1.80 mg/L) For cooling water with molybdenum-based treatment FerroMo Method ™ Enter the stored Press: Fill a 50-mL Add the contents of 38 ENTER program number for graduated mixing one FerroMo Iron The display will show iron (Fe).
Page 204 IRON, TOTAL, continued Insert the blank in the Press: After the timer Press: ZERO READ cell holder. Tightly beeps, place the The cursor will move to The cursor will move to cover the sample cell prepared sample in the the right, then the the right, then the result with the instrument cap.
Page 205 IRON, TOTAL, continued mL of standard added. d) If these increases do not occur, see Standard Additions in Section 1 for more Information. Standard Solution Method Prepare a 0.4 mg/L iron working solution as follows: a) Pipet 1.00 mL of Iron Standard Solution, 100 mg/L Fe, into a 250-mL volumetric flask.
Page 206 Pipet Tips, for 19700-01 Pipet ..............50/pkg..21856-96 Pipet Tips, for 19700-01 Pipet ............1000/pkg..21856-28 Pipet, volumetric, Class A, 1.00 mL............each..14515-35 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 207: Iron, Total, Tptz Method
Method 8112 IRON, TOTAL (0 to 1.80 mg/L) For water, wastewater, and seawater TPTZ Method (Powder Pillows or AccuVac Ampuls) Using Powder Pillows Enter the stored Press: Fill a sample cell Add the contents of 39 ENTER program number for iron with 10 mL of sample.
Page 208 IRON, TOTAL, continued Press: Fill a second sample Place the blank in the Press: ZERO cell with 10 mL of cell holder. Tightly TIMER ENTER The cursor will move sample (the blank). cover the sample cell A three-minute reaction with the instrument cap. to the right, then the period will begin.
Page 209 IRON, TOTAL, continued Using AccuVac Ampuls Enter the stored Press: Fill a sample cell Fill a TPTZ Iron 39 ENTER program number for iron with at least 10 mL of AccuVac Ampul The display will show (Fe)- AccuVac Ampuls. sample (the blank). with sample.
Page 210 IRON, TOTAL, continued When the timer Press: READ beeps, place the The cursor will move to prepared sample into the the right, then the result cell holder. Tightly in mg/L iron will cover the ampul with the be displayed. instrument cap. Note: Standard Adjust may be performed using a prepared standard (see...
Page 211 IRON, TOTAL, continued d) Add two additional 0.1-mL aliquots of standard, measuring the concentration after each addition. The iron concentration should increase by 0.25 mg/L for each 0.1- mL addition of standard. e) If these increases do not occur, see Standard Additions in Section 1 for more information.
Page 212 IRON, TOTAL, continued Estimated Detection Limit The estimated detection limit for program 39 is 0.04 mg/L Fe. For more information on the estimated detection limit, see Section 1. Interferences Interfering Substance Interference Levels and Treatments Cadmium Greater than 4.0 mg/L Chromium ( Greater than 0.25 mg/L Chromium (...
Page 213 Pipet TenSette, 0.1 to 1.0 mL ..............each ..19700-01 Pipet Tips, for 19700-01 TenSette Pipet ..........50/pkg ..21856-96 Pipet, volumetric, Class A, 1.00 mL ............each ..14515-35 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 215: Manganese, High Range Periodate Oxidation Method
Method 8034 MANGANESE, High Range (0 to 20.0 mg/L) For water and wastewater Periodate Oxidation Method USEPA approved for reporting wastewater analysis (digestion is required; see Section 2) Enter the stored Press: Fill a sample cell Place the blank into 41 ENTER program number for with 10 mL of sample...
Page 216 MANGANESE, High Range, continued Place the prepared Press: READ sample into the cell The cursor will move to holder. Tightly cover the the right, then the result sample cell with the in mg/L manganese will instrument cap. be displayed. Note: Standard Adjust may be performed using a prepared standard (see Section 1).
Page 217 MANGANESE, High Range, continued e) If these increases do not occur, see Standard Additions in Section 1 for troubleshooting information. Standard Solution Method Prepare a 5.0 mg/L manganese standard solution by pipetting (use a TenSette or Class A volumetric pipet) 5.00 mL of Manganese Standard Solution, 1000 mg/L Mn, into a 1000-mL volumetric flask.
Page 218 Pipet, volumetric, Class A, 5.00 mL............each..14515-37 Pipet, volumetric, Class A, 1.00 mL............each..14515-35 Pipet Filler, safety bulb ................each..14651-00 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 219: Molybdenum, Molybdate, Low Range Ternary Complex Method
Method 8169 MOLYBDENUM, MOLYBDATE, Low Range (0 to 3.00 mg/L) Ternary Complex Method For boiler and cooling tower waters Enter the stored Press: Fill a 25-mL mixing Add the contents of 47 ENTER program number for graduated cylinder with one Molybdenum 1 The display will show molybdate molybdenum.
Page 220 MOLYBDENUM, MOLYBDATE, LR, continued Insert the blank into Press: Place the developed Press: ZERO READ the cell holder. Tightly sample into the cell The cursor will move to The cursor will move to cover the sample cell holder. Tightly cover the the right, then the the right, then the result with the instrument cap.
Page 221 MOLYBDENUM, MOLYBDATE, LR, continued mL graduated mixing cylinder. Dilute to the mark with deionized water and mix thoroughly. Analyze 20 mL of this solution according to the procedure. Method Performance Precision In a single laboratory using standard solutions of 2.00 mg/L Mo and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of ±0.009 mg/L Estimated Detection Limit...
Page 222 MOLYBDENUM, MOLYBDATE, LR, continued Table 1 Negative Interferences (continued) Level above which it interferes (mg/L) Positive Interferences Carbonate 1,325 Silica Benzotriazole Morpholine Read molybdenum concentration immediately after the completion of the two-minute reaction period. Table 2 No Interference Highest Concentration Tested (mg/L) Zinc Calcium Magnesium...
Page 223 MOLYBDENUM, MOLYBDATE, LR, continued Large interferences are caused by some biocides used in cooling tower samples. Hach recommends testing the ternary complex procedure on molybdenum standards containing the specific biocides in use to determine if the ternary complex method will work with these samples.
Page 224 Pipet, volumetric, 10.00 mL, Class A............each..14515-38 Pipet Filler, safety bulb .................. each..14651-00 PourRite Ampule Breaker................each..24846-00 For Technical Assistance, Price and Ordering In the U.S.A. call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 225: Nitrogen, Free Ammonia And Chloramine (Mono) Indophenol Method
Nitrogen, Free Ammonia and Chloramine (Mono) Method 10200 Indophenol Method (0–4.50 mg/L Cl and 0–0.50 mg/L NH –N) For finished chloraminated drinking water For the most accurate chloramine results, determine a reagent Note: blank for each new lot of reagent using deionized water instead of sample.
Page 226 Nitrogen, Free Ammonia and Chloramine (Mono), continued Slot Slot Cap the reagent Cap the cell and Press: When the timer bottle to maintain mix. expires, place the TIMER ENTER reagent performance and Monochloramine cell Note: If the sample A five-minute reaction stability.
Page 227 Nitrogen, Free Ammonia and Chloramine (Mono), continued Add the contents Cap and shake the Press: After the timer has of one pillow of cell about 20 seconds to expired, press: TIMER ENTER EXIT Monochlor F to the cell dissolve the reagent. A five-minute reaction for the Free Ammonia A green color will form...
Page 228 Nitrogen, Free Ammonia and Chloramine (Mono), continued Sampling and Storage Collect samples in clean glass bottles. Most reliable results are obtained when samples are analyzed as soon as possible after collection. Color Development Time Test results are strongly influenced by sample temperature. Both reaction periods in the procedure are the same and depend on the temperature of the sample.
Page 229 Nitrogen, Free Ammonia and Chloramine (Mono), continued Substance Level Tested Aluminum 0.2 mg/L Al Chloride 1200 mg/L Cl Copper 1 mg/L Cu Iron 0.3 mg/L Fe Manganese 0.05 mg/L Mn Nitrate 10 mg/L NO –N Nitrite 1 mg/L NO –N Phosphate 2 mg/L –PO Silica...
Page 230 Nitrogen, Free Ammonia and Chloramine (Mono), continued 4. Dilute to volume with organic-free water, cap and mix thoroughly. This is a 2.00 mg/L buffered ammonia standard. 5. Pipet 50.0 mL of the buffered ammonia standard into a clean 100-mL beaker. Add a stir bar. 6.
Page 231 ± 0.01 mg/L N for seven replicates. Estimated Detection Limit The estimated detection limit for program 46 is 0.02 mg/L N. For more information on the estimated detection limit, see Section 1 of the DR/850 or DR/890 Procedure Manual.
Page 232 Nitrogen, Free Ammonia and Chloramine (Mono), continued Summary of Method Monochloramine (NH Cl) and “free ammonia” (NH and NH can exist in the same water sample. Added hypochlorite combines with free ammonia to form more monochloramine. In the presence of a cyanoferrate catalyst, monochloramine in the sample reacts with a substituted phenol to form an intermediate monoimine compound.
Page 233 Nitrogen, Free Ammonia and Chloramine (Mono), continued OPTIONAL APPARATUS Description Per Test Unit Cat. No. Ampule Breaker Kit ................each....21968-00 Beaker, 100 mL, Polypropylene............each....1080-42 Beaker, 100 mL, Glass .................each....500-42H Cylinder, 50 mL, mixing ..............each....20886-41 Flask, Volumetric, Class A, 100 mL ............each....14574-42 Pipet Filler, Safety Bulb ...............each....14651-00 ®...
Page 235: Nitrate, High Range, Cadmium Reduction Method
Method 8039 NITRATE, High Range (0 to 30.0 mg/L NO For water, wastewater, and seawater Cadmium Reduction Method (Using Powder Pillows or AccuVac Ampuls) Using Powder Pillows Enter the stored Press: Fill a sample cell Add the contents of 51 ENTER program number for with 10 mL of sample.
Page 236 NITRATE, High Range, continued Press: After the timer beeps, Fill another cell with Place the blank into the display will show: 10 mL of sample (the the cell holder. Tightly TIMER ENTER 5:00 TIMER 2 blank). Wipe off any cover the sample cell A one-minute reaction fingerprints or liquid.
Page 237 NITRATE, High Range, continued Using AccuVac Ampuls Enter the stored Press: Collect at least 40 Press: 50 ENTER program number for mL of sample in a TIMER ENTER The display will show high range nitrate 50-mL beaker. Fill a mg/L, NO3-N and the A one-minute mixing nitrogen (NO ¯–N)
Page 238 NITRATE, High Range, continued Place the AccuVac Press: READ Ampul into the cell The cursor will move to holder. Tightly cover the the right, then the result ampul with the in mg/L NO -N (or instrument cap. alternate form) will be displayed.
Page 239 If these increases do not occur, see Standard Additions (Section 1) for more information. Standard Solution Method Use a Hach Nitrate-Nitrogen Standard Solution, 10.0 mg/L NO N, listed under Optional Reagents as the sample and perform the procedure as described above.
Page 240 NITRATE, High Range, continued Estimated Detection Limit The estimated detection limit for program 50 is 0.5 mg/L NO and 0.8 mg/L NO -N for program 51. For more information on the estimated detection limit, see Section 1. Interferences Interfering Interference Levels and Treatments Substance Chloride Chloride concentrations above 100 mg/L will cause low results.
Page 241 PourRite Ampule Breaker ................each ..24846-00 Thermometer, –20 to 110 °C, non-mercury ..........each ..26357-02 For Technical Assistance, Price and Ordering In the U.S.A. call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you. Contact Hach for larger sizes.
Page 243: Nitrate, Low Range, Cadmium Reduction Method
Method 8192 NITRATE, Low Range (0 to 0.50 mg/L NO For water, wastewater and seawater Cadmium Reduction Method Enter the stored Press: Fill a 25-mL Add the contents of 55 ENTER program number for low graduated mixing one NitraVer 6 Nitrate The display will show range nitrate nitrogen cylinder to the 15-mL...
Page 244 NITRATE, Low Range, continued Press: When the timer When the timer Add the contents of beeps, the display will beeps, pour 10 mL of the one NitriVer 3 Nitrite TIMER ENTER show: 2:00 TIMER 2 sample into a Reagent Powder Pillow A 3-minute reaction sample cell.
Page 245 NITRATE, Low Range, continued Press: Note: See Pollution READ Prevention and Waste The cursor will move to Management for proper the right, then the result disposal of cadmium. in mg/L NO (or alternate form) will be displayed. Note: Standard Adjust may be performed using a prepared standard (see Section 1).
Page 246 NITRATE, Low Range, continued Accuracy Check Standard additions Method a) Fill three 25-mL graduated mixing cylinders with 15 mL of sample. b) Snap the neck off a Nitrate Nitrogen Ampule Standard Solution, 12.0 mg/L NO c) Using the TenSette Pipet, add 0.1, 0.2, and 0.3 mL of the standard to the three samples.
Page 247 NITRATE, Low Range, continued Estimated Detection Limit The estimated detection limit for program 55 is 0.01 mg/L NO N. For more information on the estimated detection limit, see Section 1. Interferences Interfering Interference Levels and Treatments Substance Calcium 100 mg/L Chloride Chloride concentrations above 100 mg/L will cause low results.
Page 248 Nitrate at these levels can also be determined directly using the Nitrate Ion Selective Electrode (Cat. No. 23488-00). For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you. Contact Hach for larger sizes...
Page 249: Nitrite, Low Range Diazotization Method
Method 8507 NITRITE, Low Range (0 to 0.350 mg/L NO For water, wastewater, seawater Diazotization Method (Powder Pillows or AccuVac Ampuls); USEPA approved for reporting wastewater and drinking water analyses. Enter the stored Press: Fill a sample cell Add the contents of 60 ENTER program number with 10 mL of sample.
Page 250 NITRITE, Low Range, continued Press: When the timer Wipe the outside of Press: ZERO beeps, fill an empty the sample cell with a TIMER ENTER The cursor will move to sample cell with 10 mL towel. Place the blank A 15-minute reaction the right, then the of sample (the blank).
Page 251 NITRITE, Low Range, continued Using AccuVac Ampuls Enter the stored Press: Collect at least Quickly invert the 62 ENTER program number 40 mL of sample in a ampul several times to The display will show for nitrite nitrogen 50-mL beaker. Fill a mix.
Page 252 NITRITE, Low Range, continued Place the AccuVac Press: READ Ampul into the cell The cursor will move to holder. Tightly cover the the right, then the result ampul with the in mg/L nitrite nitrogen instrument cap. will be displayed. Sampling and Storage Collect samples in clean plastic or glass bottles.
Page 253 Estimated Detection Limit The estimated detection limit for programs 60 and 62 is 0.005 mg/L NO -N. For more information on derivation and use of Hach’s estimated detection limit, see Section 1. Interferences Interfering Interference Levels Substance Antiminous ions...
Page 254 Pipet, volumetric, Class A, 10.00 mL............each..14515-38 Pipet Filler, safety bulb .................. each..14651-00 Thermometer, –20 to 110 °C................each..26357-02 For Technical Assistance, Price and Ordering In the U.S.A. call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 255: Nitrite, Low Range, Test 'N Tube Diazotization Method
Method 10019 NITRITE, Low Range, Test ‘N Tube (0–0.500 mg/L NO Diazotization Method For water, wastewater, and seawater USEPA approved for wastewater analysis Enter the stored Press: Insert the COD/TNT Fill a Test ‘N Tube 63 ENTER ® program number Adapter into the cell NitriVer 3 Nitrite vial...
Page 256 Remove suspended solids by filtration. Accuracy Check Standard Solution Method Pipet 5.00 mL of a fresh Hach standard, 250 mg/L as NO -N into a Class A 250-mL volumetric flask. Dilute to the line with deionized water to make a 5.00-mg/L intermediate standard.
Page 257 ±0.004 mg/L NO Estimated Detection Limit The estimated detection limit for program 63 is 0.006 mg/L NO -N. For more information on derivation and use of Hach’s estimated detection limit, see Section 1. Interferences Interfering...
Page 258 Flask, volumetric, 250 mL................each..14574-46 Flask, volumetric, 500 mL................each..14574-49 Pipet, volumetric, Class A, 10.00 mL............each..14515-38 For Technical Assistance, Price and Ordering In the U.S.A. call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you. * Not available separately.
Page 259: Nitrogen, Ammonia Salicylate Method
Method 8155 NITROGEN, AMMONIA (0 to 0.50 mg/L NH For water, wastewater, seawater Salicylate Method Enter the stored Press: Fill a sample cell Fill a second sample 64 ENTER program number with 10 mL of deionized cell with 10 mL of The display will show for ammonia nitrogen water (the blank).
Page 260 NITROGEN, AMMONIA, continued After the timer Press: Place the prepared Press: ZERO READ beeps, place the blank sample into the cell The cursor will move to The cursor will move to into the cell holder. holder. Tightly cover the the right, then the the right, then the result Tightly cover the sample sample cell with the...
Page 261 NITROGEN, AMMONIA, continued Accuracy Check Standard Additions Method a) Fill three 25-mL mixing cylinders with 20 mL of sample. b) Use the TenSette Pipet to add 0.1, 0.2, and 0.3 mL of Ammonium Nitrogen Standard, 10 mg/L as NH -N to the three samples.
Page 262 Turbidity and sample color will give erroneous high values. Samples with severe interferences require distillation. Albuminoid nitrogen samples also require distillation. Hach recommends the distillation procedure using the Hach General Purpose Distillation Set. See the Optional Apparatus list. Summary of Method Ammonia compounds combine with chlorine to form monochloramine.
Page 263 Pipet, volumetric, Class A, 2.0 mL .............each ..14515-36 PourRite Ampule Breaker Kit ..............each ..24846-00 Thermometer, –20 to 110 °C ...............each ..26357-02 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 265: Nitrogen, Ammonia, Low Range, Test 'N Tube Salicylate Method
Method 10023 NITROGEN, AMMONIA, Low Range, Test ‘N Tube (0 to 2.50 mg/L NH Salicylate Method For water, wastewater, and seawater Enter the stored Press: Insert the COD/TNT Remove the caps 66 ENTER program number for low Adapter into the cell from 2 AmVer Diluent The display will show range nitrogen, ammonia...
Page 266 NITROGEN, AMMONIA, Low Range, Test 'N Tube, continued Wipe the outside of Press: Place the prepared Tightly cover the ZERO the vials with a towel. sample in the adapter. sample cell with the The cursor will move to After the timer beeps, instrument cap.
Page 267 NITROGEN, AMMONIA, Low Range, Test 'N Tube, continued c) Analyze each sample as described above. The nitrogen concentration should increase 0.20 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 To check accuracy, use a 1.0 mg/L Nitrogen, Ammonia Standard Solution listed under Optional Reagents.
Page 268 Turbidity and color will give erroneous high values. Samples with severe interferences require distillation. Hach recommends the distillation procedure using the Hach General Purpose Distillation Set. See Optional Apparatus at the end of this procedure.
Page 269 Ampule Breaker Kit, PourRite ..............each ..24846-00 Thermometer, –20 to 110 °C, non-mercury ..........each ..26357-02 Thermometer, –10 to 260 °C, non-mercury ..........each ..26357-01 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 271: Nitrogen, Ammonia, High Range, Test 'N Tube, Salicylate Method
Method 10031 NITROGEN, AMMONIA, High Range, Test ‘N Tube (0 to 50 mg/L NH For water, wastewater, and seawater Salicylate Method Enter the stored Press: Insert the COD/TNT Remove the caps 67 ENTER program number for Adapter into the cell from 2 AmVer Diluent The display will show nitrogen, ammonia, high...
Page 272 NITROGEN, AMMONIA, High Range, Test 'N Tube, continued Clean the outside of Press: Place the prepared Tightly cover the ZERO the vial with a towel. sample in the adapter. vial with the instrument The cursor will move to After the timer beeps, cap.
Page 273 NITROGEN, AMMONIA, High Range, Test 'N Tube, continued Sampling and Storage Collect samples in clean plastic or glass bottles. Best results are obtained with immediate analysis. If chlorine is known to be present, add one drop of 0.1 N sodium thiosulfate for each 0.3 mg/L Cl in a one liter sample.
Page 274 3. Filter the sample through folded filter paper. Use the filtered solution in step 4. Turbidity and color Give erroneous high values. Samples with severe interferences require distillation. Hach recommends the distillation procedure using the Hach General Purpose Distillation Set.
Page 275 NITROGEN, AMMONIA, High Range, Test 'N Tube, continued Summary of Method Ammonia compounds combine with chlorine to form monochloramine. Monochloramine reacts with salicylate to form 5- aminosalicylate. The 5-aminosalicylate is oxidized in the presence of a sodium nitroprusside catalyst to form a blue-colored compound. The blue color is masked by the yellow color from the excess reagent present to give a green-colored solution.
Page 276 Pipet Tips, for 19700-01 TenSette Pipet ..........1000/pkg..21856-28 ™ PourRite Ampule Breaker ............... each..24846-00 Sample Cell, 10-20-25 mL, w/cap ............6/pkg..24019-06 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 277: Nitrogen, Total Inorganic, Test 'N Tube ™ , Titanium Trichloride Reduction Method
Method 10021 NITROGEN, Total Inorganic, Test ‘N Tube ™ (0 to 25.0 mg/L N) Titanium Trichloride Reduction Method For water, wastewater, and seawater Requires Centrifuge Enter the stored Press: Insert the COD/TNT Pipet 1 mL of Total 68 ENTER program number for Adapter into the cell Inorganic Nitrogen The display will show...
Page 278 NITROGEN, TOTAL INORGANIC, Test 'N Tube, continued Remove the caps Using a funnel, add Using a funnel, add Cap the vials tightly from 2 AmVer Diluent the contents of one the contents of one and shake thoroughly to Reagent Test ‘N Tubes Ammonia Salicylate Ammonia Cyanurate dissolve the powder.
Page 279 NITROGEN, TOTAL INORGANIC, Test 'N Tube, continued Place the prepared Tightly cover the Press: READ sample in the adapter. sample cell with the The cursor will move to instrument cap. Push straight down on the right, then the result the top of the vial until it in mg/L total inorganic seats solidly into the nitrogen will be...
Page 280 NITROGEN, TOTAL INORGANIC, Test 'N Tube, continued d) Analyze each sample as described in the procedure; use a 1-mL aliquot of the prepared sample in Step 5. The nitrogen concentration should increase about 1.8 to 1.9 mg/L for each 0.1 mL of standard added. e) If these increases do not occur, see Standard Additions in Section 1 for more information.
Page 281 NITROGEN, TOTAL INORGANIC, Test 'N Tube, continued In a single laboratory, using a standard solution of 20.0 mg/L N and 2 representative lots of reagent with the instrument, a single operator obtained a mean recovery of 14.6 mg/L with a standard deviation of ±...
Page 282 NITROGEN, TOTAL INORGANIC, Test 'N Tube, continued REQUIRED REAGENTS Total Inorganic Nitrogen Pretreatment Reagent Set (TiCl Reduction) (25 tests)..26049-45 Includes: (1) 26051-50, (1) 2040-59, (50) TIN Pretreatment Diluent Vials AmVer ™ Reagent Set for Nitrogen, Ammonia, Low Range (25 tests) ......26045-45 ™...
Page 283 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 Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 285: Oxygen Demand, Chemical, Manganese Iii Digestion Method
Method 10067 OXYGEN DEMAND, CHEMICAL (20 to 1,000 mg/L) For water and wastewater Manganese III Digestion Method (without chloride removal) Enter the stored Press: Homogenize If chloride is not 18 ENTER program number for 100 mL of sample for present in significant The display will show †...
Page 286 OXYGEN DEMAND, CHEMICAL, continued 2:00 minutes PREPARE BLANK Prepare a blank (see Place the vials in Remove the vials Remove the vials note) by substituting the DRB 200 Reactor and place them in a from the water and wipe 0.50 mL of deionized that is preheated to 150 cooling rack for two with a clean, dry...
Page 287 OXYGEN DEMAND, CHEMICAL, continued Insert the Place the blank in Tightly cover the If the chloride COD/TNT Adapter into the sample cell adapter. sample cell with the removal was done, make the cell holder by instrument cap. sure the filter disc is not Push straight down on rotating the adapter until suspended in the middle...
Page 288 ±23 mg/L COD. Estimated Detection Limit (EDL) The EDL for program 18 is 14 mg/L COD. For more information on derivation and use of Hach’s estimated detection limit, see Section 1. Interferences Inorganic materials may also be oxidized by trivalent manganese and constitute a positive interference when present in significant amounts.
Page 289 OXYGEN DEMAND, CHEMICAL, continued routine samples with and without the chloride removal, then compare results. Other inorganic interferences (i.e., nitrite, ferrous iron, sulfide) are not usually present in significant amounts. If necessary, these interferences can be corrected for after determining their concentrations with separate methods and adjusting the final COD test results accordingly.
Page 290 DRB 200 Reactor, 110 V, 9 x 16 mm and 2 x 20 mm ........LTV082.53.30001 DRB 200 Reactor, 220 V, 9 x 16 mm and 2 x 20 mm ........LTV082.52.30001 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 291: Organic Carbon, Total, Low Range, Direct Method
Method 10129 ORGANIC CARBON, TOTAL, Low Range (0.0–20.0 mg/L C) Direct Method For water, drinking water, and wastewater HRS MIN SEC HRS MIN SEC Turn on the Use a graduated Add 0.4 mL of Place the flask on a DRB 200 reactor. Heat cylinder to add 10 mL of Buffer Solution, pH 2.0.
Page 292 ORGANIC CARBON, TOTAL, Low Range, continued Lower one unopened Cap the vial Carefully remove Insert the ampule into each Acid assemblies tightly and the vial assemblies from COD/TNT Adapter into Digestion vial. When the place them in the the reactor. Place them the cell holder by score mark on the reactor for 2 hours at...
Page 293 ORGANIC CARBON, TOTAL, Low Range, continued Tightly cover the Press: Wipe the sample Place the sample ZERO vial assembly with the vial assembly with a vial assembly in the The cursor will move to instrument cap. damp towel, followed by adapter.
Page 294 ORGANIC CARBON, TOTAL, Low Range, continued Accuracy Check Standard Solutions Method a. Prepare a 1000 mg/L organic carbon stock standard by dissolving 2.1254 g dry primary standard Potassium Acid Phthalate in Organic-Free Reagent Water and dilute to 1000 mL. This stock standard is stable for about 1 month at room temperature.
Page 295 ORGANIC CARBON, TOTAL, Low Range, continued Method Performance Precision In a single laboratory, using a standard solution of 9.0 mg/L C and one lot of reagents, a single operator obtained a standard deviation of ±0.5 mg/L C. Estimated Detection Limit The estimated detection limit for Method 10129 is 0.3 mg/L C.
Page 296 ORGANIC CARBON, TOTAL, Low Range, continued Table 1 Non-interfering Substances (Continued) Substance Maximum Level Tested Silica 100 mg/L SiO Sulfate 5000 mg/L SO Sulfide 20 mg/L S Sulfite 50 mg/L SO Zinc 5 mg/L If the sample contains greater than 600 mg/L CaCO alkalinity, lower the sample pH to less than 7 before testing by adding sulfuric acid solution.
Page 297 ORGANIC CARBON, TOTAL, Low Range, continued REQUIRED APPARATUS Description Qty/Test Unit Cat. No. Cylinder, graduated, 10-mL ........... 1....each ....508-38 DRB 200 Reactor, 110 V, 15 x 16 mm tubes ..........LTV082.53.40001 DRB 200 Reactor, 220 V, 15 x 16 mm tubes ..........LTV082.52.40001 Flask, Erlenmeyer, 50-mL............
Page 299: Organic Carbon, Total, Mid Range, Direct Method
Method 10173 ORGANIC CARBON, TOTAL, Mid Range (15–150 mg/L C) Direct Method For wastewater and industrial waters HRS MIN SEC HRS MIN SEC Turn on the Use a graduated Add 0.4 mL of Place the flask on a DRB 200 reactor. Heat cylinder to add 10 mL of Buffer Solution, pH 2.0.
Page 300 ORGANIC CARBON, TOTAL, Mid Range, continued Lower one unopened Cap the vial Carefully remove Insert the ampule into each Acid assemblies tightly and the vial assemblies from COD/TNT Adapter into Digestion vial. When the place them in the the reactor. Place them the cell holder by score mark on the reactor for 2 hours at...
Page 301 ORGANIC CARBON, TOTAL, Mid Range, continued Tightly cover the Press: Wipe the sample Place the sample ZERO vial assembly with the vial assembly with a vial assembly in the The cursor will move to instrument cap. damp towel, followed by adapter.
Page 302 ORGANIC CARBON, TOTAL, Mid Range, continued Sampling and Storage Collect samples in clean glass bottles. Rinse the sample bottle several times with the sample to be collected. Fill the bottle with minimum headspace before capping. Test samples as soon as possible.
Page 303 ORGANIC CARBON, TOTAL, Mid Range, continued Method Performance Precision mg/L C 95% Confidence Limits ± 5 mg/L C ± 6 mg/L ± 7 mg/L ± 4 mg/L ± 6 mg/L Estimated Detection Limit Use Method Number 10173 to test TOC levels below 15 mg/L C. Sensitivity At mid-range, the sensitivity, expressed as the concentration change per 0.010 absorbance change, is 1.9 mg/L C.
Page 304 ORGANIC CARBON, TOTAL, Mid Range, continued Table 1 Non-interfering Substances (Continued) Substance Maximum Level Tested Monochloramine 14 mg/L NH Cl as Cl Nitrite 500 mg/L NO Ozone 2 mg/L O Phosphate 3390 mg/L PO Silica 100 mg/L SiO Sulfate 5000 mg/L SO Sulfide 20 mg/L S Sulfite...
Page 305 ORGANIC CARBON, TOTAL, Mid Range, continued Instrument Setup This procedure will add the current method as a new Hach program to your DR/850 or DR/890. Line Number Entry Line Number Entry 1. Turn the instrument on by pressing the key.
Page 306 ORGANIC CARBON, TOTAL, Mid Range, continued REQUIRED REAGENTS Total Organic Carbon Direct Method Mid Range Test ’N Tube Reagent Set ..............50 vials..28159-45 Includes: Quantity Required Description Per Test Unit Cat. No......* Acid Digestion Solution Vials, Mid Range TOC ....1 ..... 50/pkg Buffer Solution, Sulfate .............
Page 307: Organic Carbon, Total, High Range, Direct Method
Method 10128 ORGANIC CARBON, TOTAL, High Range (20–700 mg/L C) Direct Method For wastewater and industrial waters HRS MIN SEC HRS MIN SEC Turn on the Use a graduated Add 0.4 mL of Place the flask on a DRB 200 reactor. Heat cylinder to add 10 mL of Buffer Solution, pH 2.0.
Page 308 ORGANIC CARBON, TOTAL, High Range, continued Lower one unopened Cap the vial Carefully remove Insert the ampule into each Acid assemblies tightly and the vial assemblies from COD/TNT Adapter into Digestion vial. When the place them in the the reactor. Place them the cell holder by score mark on the reactor for 2 hours at...
Page 309 ORGANIC CARBON, TOTAL, High Range, continued Tightly cover the Press: Wipe the sample Place the sample ZERO vial assembly with the vial assembly with a vial assembly in the The cursor will move to instrument cap. damp towel, followed by adapter.
Page 310 ORGANIC CARBON, TOTAL, High Range, continued Accuracy Check Standard Solutions Method a. Prepare a 1000 mg/L organic carbon stock standard by dissolving 2.1254 g dry primary standard Potassium Acid Phthalate in Organic-Free Reagent Water and dilute to 1000 mL. This stock standard is stable for about 1 month at room temperature.
Page 311 ORGANIC CARBON, TOTAL, High Range, continued Method Performance Precision In a single laboratory, using a standard solution of 360 mg/L C and one lot of reagents, a single operator obtained a standard deviation of ±8 mg/L C. Estimated Detection Limit Use Method Number 10129 to test TOC levels below 20 mg/L C.
Page 312 ORGANIC CARBON, TOTAL, High Range, continued Table 1 Non-interfering Substances (Continued) Substance Maximum Level Tested Silica 100 mg/L SiO Sulfate 5000 mg/L SO Sulfide 20 mg/L S Sulfite 50 mg/L SO Zinc 5 mg/L If the sample contains greater than 600 mg/L CaCO alkalinity, lower the sample pH to less than 7 before testing by adding sulfuric acid solution.
Page 313 ORGANIC CARBON, TOTAL, High Range, continued REQUIRED APPARATUS Cylinder, graduated, 10-mL ........... 1....each ....508-38 DRB 200 Reactor, 110 V, 15 x 16 mm tubes ..........LTV082.53.40001 DRB 200 Reactor, 220 V, 15 x 16 mm tubes ..........LTV082.52.40001 Flask, Erlenmeyer, 50-mL............1....each ....505-41 Magnetic Stirrer, 115 V, 4"...
Page 315: Oxygen Demand, Chemical, Manganese Iii Digestion Method
Method 10067 OXYGEN DEMAND, CHEMICAL (20 to 1,000 mg/L) For water and wastewater Manganese III Digestion Method (with chloride removal) Enter the stored Press: Homogenize Chloride Removal 18 ENTER program number for 100 mL of sample for Procedure The display will show Manganese III COD.
Page 316 OXYGEN DEMAND, CHEMICAL, continued PREPARE BLANK Using an automatic Cap the cell tightly Prepare a blank (see If not already on, dispenser or TenSette and invert it several note) by repeating Steps turn on the DRB 200 Pipet, add 1.0 mL of times.
Page 317 OXYGEN DEMAND, CHEMICAL, continued Table 1 Dilution Table (for use with Chloride Removal Procedure Only) Sample (mL) Deionized Water (mL) Range (mg/L COD) Multiplication Factor 30-1500 60-3000 180-9000 360-18000 All dilutions require that the ratio of sample to sulfuric acid remain at 9:1. For other dilutions that are not listed in Table 1, simply add the sample volume + deionized water and divide by the sample volume to obtain the multiplication factor.
Page 318 OXYGEN DEMAND, CHEMICAL, continued Close the vacuum Open the VPD Use forceps to Remove the Mn III regulator valve regulator valve to remove the filter from COD vial from the completely to achieve release the vacuum. the top of each CRC. vacuum chamber and full vacuum.
Page 319 OXYGEN DEMAND, CHEMICAL, continued 2:00 minutes Place the vials in Remove the vials Remove the vials Insert the the DRB 200 Reactor and place them in a from the water and wipe COD/TNT Adapter into that is preheated to 150 cooling rack for two with a clean, dry the cell holder by...
Page 320 OXYGEN DEMAND, CHEMICAL, continued Place the blank in Tightly cover the If the chloride Place the sample in the sample cell adapter. sample cell with the removal was done, make the adapter. instrument cap. sure the filter disc is not Push straight down on Push straight down on suspended in the middle...
Page 321 ±23 mg/L COD. Estimated Detection Limit (EDL) The EDL for program 18 is 14 mg/L COD. For more information on derivation and use of Hach’s estimated detection limit, see Section 1. Interferences Inorganic materials may also be oxidized by trivalent manganese and constitute a positive interference when present in significant amounts.
Page 322 OXYGEN DEMAND, CHEMICAL, continued routine samples with and without the chloride removal, then compare results. Other inorganic interferences (i.e., nitrite, ferrous iron, sulfide) are not usually present in significant amounts. If necessary, these interferences can be corrected for after determining their concentrations with separate methods and adjusting the final COD test results accordingly.
Page 323 DRB 200 Reactor, 110 V, 9 x 16 mm and 2 x 20 mm ........LTV082.53.30001 DRB 200 Reactor, 220 V, 9 x 16 mm and 2 x 20 mm........LTV082.52.30001 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 325: Oxygen, Dissolved, High Range Hrdo Method
Method 8166 OXYGEN, DISSOLVED, High Range (0 to 15.0 mg/L O HRDO Method For water and wastewater Enter the stored Press: Fill a sample cell Fill a High Range 70 ENTER program number (the blank) with at least Dissolved Oxygen The display will show for dissolved oxygen, 10 mL of sample.
Page 326 OXYGEN, DISSOLVED, High Range, continued Press: Place the AccuVac Press: ZERO READ ampul into the cell The cursor will move to The cursor will move to holder. Tightly cover the the right, then the the right, then the result ampul with the display will show: in mg/L O will...
Page 327 OXYGEN, DISSOLVED, High Range, continued Accuracy Check The results of this procedure may be compared with the results of a dissolved oxygen meter (Cat. No. 51815-01). Method Performance Precision In a single laboratory, using a standard solution of 8.0 mg/L O determined by the Winkler method and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of...
Page 328 Dissolved Oxygen Reagent Set (Digital Titrator Method) ....50 tests..22722-00 Dissolved oxygen may also be determined by titrimetric methods. Request Publication 8042 for additional information. For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 329: Oxygen, Dissolved, Low Range Indigo Carmine Method
Method 8316 OXYGEN, DISSOLVED, Low Range (0 to 1000 µg/L O ) For boiler feedwater Indigo Carmine Method (Using AccuVac Ampuls) Enter the stored Press: Fill a sample cell Place the blank into 71 ENTER program number for low with at least 10 mL of the cell holder.
Page 330 ±2 µg/L O . For more information on Hach’s precision statement, see Section 1. Estimated Detection Limit The estimated detection limit for program #71 is 10 µg/L O .
Page 331 Sample Cell, 10-20-25 mL, w/cap ........1 ......6/pkg ..24019-06 OPTIONAL REAGENTS AND APPARATUS AccuVac Snapper Kit ..................each ..24052-00 Sodium Hydrosulfite, technical grade............500 g ....294-34 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 333: Ozone Indigo Method
Method 8311 OZONE (0 to 0.25 mg/L O , 0 to 0.75 mg/L O or 0 to 1.50 mg/L O For water Indigo Method (Using AccuVac Ampuls) Enter the stored Press: Gently collect at least Collect at least 40 72 ENTER program number for for low range ozone 40 mL of sample in a...
Page 334 ±0.01, ±0.02 and ±0.02 mg/L O for the low, mid and high range tests, respectively. For more information on Hach’s precision statement, see Section 1.
Page 335 Water, deionized ............varies ......4 L ....272-56 REQUIRED APPARATUS Beaker, 50 mL ...............2 ......each ...500-41H OPTIONAL APPARATUS AccuVac Snapper Kit ..................each ..24052-00 AccuVac Ampule sampler................each ..24051-00 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 337: Ph, Colorimetric Ph Determination Using Phenol Red
Method 10076 (6.5 to 8.5 pH units) Colorimetric pH Determination Using Phenol Red For water and wastewater Enter the stored Press: Fill a sample cell Place the blank in the 75 ENTER program number for the with 10 mL of sample cell holder.
Page 338 continued Press: READ The cursor will move to the right, then the result in pH units will be displayed. Note: Use of the Standard Adjust feature is highly recommended. See Accuracy Check. Note: Any reading below 6.5 pH units will be erroneous.
Page 339 7.0 Buffer Solution ...............500 mL....12222-49 OPTIONAL APPARATUS Description Units Cat. No. Thermometer, -20 to 110 °C, Non-Mercury..........each....26357-02 For Technical Assistance, Price and Ordering In the U.S.A. call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 341: Phosphonates Persulfate Uv Oxidation Method
Method 8007 PHOSPHONATES (0-2.5 to 0-125 mg/L) For water, wastewater, and seawater Persulfate UV Oxidation Method Enter the stored Press: Choose the Fill a sample cell to 80 ENTER program number appropriate sample size the 10-mL mark with The display will show for phosphonates.
Page 342 PHOSPHONATES, continued Add the contents of Insert the ultraviolet Turn on the UV lamp When the timer one Potassium (UV) lamp into the to digest the prepared beeps, turn off the UV Persulfate for prepared sample. sample. lamp. Remove it from Phosphonate Powder the sample cell.
Page 343 PHOSPHONATES, continued Pour 10 mL of Add the contents of The display will When the timer sample from the cell one PhosVer 3 show: 2:00 TIMER 2 beeps, place the blank labeled as “sample” into Phosphate Reagent into the cell holder. Press: ENTER a second clean, dry...
Page 344 PHOSPHONATES, continued Table 2 Table 3 Sample Volume (mL) Phosphonate Type Conversion Factor Multiplier (chosen in Step 3) PBTC 2.84 1.050 HEDPA 1.085 EDTMPA 1.148 HMDTMPA 1.295 DETPMPA 1.207 Phosphate concentration = Instrument Reading x 1.49 Multiplier Active Phosphonate (mg/L) = Phosphate con- centration from Step 15 x Conversion Factor Sampling and Storage Collect samples in clean plastic or glass bottles that have been...
Page 345 PHOSPHONATES, continued Highly buffered samples or extreme sample pH may exceed the buffering capacity of the reagents and require sample pretreatment; see pH Interferences in Section 1. Phosphites and organophosphorus compounds other than phosphonates react quantitatively. Meta and polyphosphates do not interfere.
Page 346 Pipet, TenSette, 1-10 mL .................each ..... 19700-10 Pipet Tips, for 19700-10 Tensette Pipet..........50/pkg ..... 21997-96 Thermometer, -20 to 110 °C, Non-Mercury ..........each ....1877-01 For Technical Assistance, Price and Ordering In the U.S.A. call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 347: Phosphorus, Reactive, (Also Called Orthophosphate) Phosver 3 (Ascorbic Acid) Method
Method 8048 PHOSPHORUS, REACTIVE (0 to 2.50 mg/L PO For water, wastewater, seawater (Also called Orthophosphate) PhosVer 3 (Ascorbic Acid) Method (Powder Pillows or AccuVac Ampuls) USEPA Accepted for wastewater analysis reporting Using Powder Pillows Enter the stored Press: Fill a sample cell Add the contents of 79 ENTER program number for...
Page 348 PHOSPHORUS, REACTIVE, continued Press: Fill another sample Place the blank into Press: ZERO cell with 10 mL of the cell holder. Tightly The cursor will move to TIMER ENTER sample (the blank). cover the sample cell the right, then the A two-minute reaction with the instrument cap.
Page 349 PHOSPHORUS, REACTIVE, continued Using AccuVac Ampuls Enter the stored Press: Fill a sample cell Fill a PhosVer 3 79 ENTER program number for (the blank) with at least Phosphate AccuVac The display will show reactive phosphorus- 10 mL of sample. Ampul with sample.
Page 350 PHOSPHORUS, REACTIVE, continued Place an ampul cap Press: Place the blank into Press: ZERO securely over the tip of the cell holder. Tightly The cursor will move to TIMER ENTER the ampul. Shake the cover the sample cell the right, then the ampul for about 30 A two-minute reaction with the instrument cap.
Page 351 PHOSPHORUS, REACTIVE, continue Sampling and Storage Collect sample in plastic or glass bottles that have been cleaned with 1:1 Hydrochloric Acid Solution and rinsed with deionized water. Do not use commercial detergents containing phosphate for cleaning glassware used in this test. Analyze samples immediately after collection for best results.
Page 352 PHOSPHORUS, REACTIVE, continued Method Performance Precision In a single laboratory using a standard solution of 1.00 mg/L and two lots of reagents with the instrument, a single operator obtained a standard deviation of ±0.05 mg/L PO In a single laboratory using a standard solution of 1.00 mg/L and two representative lots of AccuVac ampuls with the instrument, a single operator obtained a standard deviation of ±0.03 mg/L PO...
Page 353 Pipet Tips, for 19700-01 ..............1000/pkg....21856-28 Pipet Filler, safety bulb ................each....14651-00 Pipet, volumetric, Class A, 4.00 mL ............each....14515-04 PourRite Ampule Breaker Kit ..............each....24846-00 Outside the U.S.A.—Contact the Hach office or distributor serving you. * Larger sizes available.
Page 355: Phosphorus, Total, (Also Called Organic And Acid Hydrolyzable) Acid Persulfate Digestion Method
Method 8190 PHOSPHORUS, TOTAL For water, wastewater, and seawater (Also called Organic and Acid Hydrolyzable) Acid Persulfate Digestion Method USEPA Accepted for reporting wastewater analysis 30:00 Measure 25 mL of Add the contents of Add 2.0 mL of Place the flask on a sample into a 50-mL one Potassium Persulfate 5.25 N Sulfuric...
Page 356 PHOSPHORUS, TOTAL, continued Cool the sample to Add 2.0 mL of Pour the sample into Note: Results of the reactive phosphorus test at room temperature. 5.0 N Sodium Hydroxide a 25-mL graduated this point will include the Solution. Swirl to mix. cylinder.
Page 357 , COD, SO , TOC) ........500 mL ..28332-49 Wastewater Influent Standard, Inorganic –N, NO –N, PO , COD, SO , TOC) ........500 mL ..28331-49 Water, deionized ................... 4 L ....272-56 * Marked Dropper Bottle - Contact Hach for larger sizes.
Page 358 Indicator Paper, 1 to 11 pH ............5 rolls/pkg ....391-33 pH Meter, Sens ™1, portable with electrode ......... each ..51700-10 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 359: Phosphorus, Acid Hydrolyzable Hydrolysis To Orthophosphate Method
Method 8180 PHOSPHORUS, ACID HYDROLYZABLE Hydrolysis to Orthophosphate Method For water, wastewater, seawater 30:00 minutes Measure 25 mL of Add 2.0 mL of Place the flask (the Cool the hot sample into a 50-mL 5.25 N Sulfuric Acid prepared sample) on a prepared sample to room erlenmeyer flask using a Solution.
Page 360 PHOSPHORUS, ACID HYDROLYZABLE, continued Add 2.0 mL of Pour the prepared 5.0 N Sodium sample into a graduated Hydroxide Solution to cylinder. Add deionized the prepared sample. water rinsings from the Swirl to mix. flask to return the volume to 25 mL. Note: Use the 1-mL Proceed with the calibrated dropper...
Page 361 PHOSPHORUS, ACID HYDROLYZABLE, continued Sampling and Storage Analyze samples immediately after collection for best results. If prompt analysis is not possible, samples may be preserved up to 48 hours by cooling to 4 °C (39 °F). Warm to room temperature before testing.
Page 362 ™1, portable with electrode ......... each ..51700-10 Thermometer, -20 to 110 °C, Non-Mercury ..........each..26357-02 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you. * Contact Hach for larger sizes.
Page 363: Phosphorus, Reactive, Phosver 3 Method, Test 'N Tube Procedure
Method 8048 PHOSPHORUS, REACTIVE (0.00 to 5.00 mg/L PO PhosVer 3 Method, Test ’N Tube Procedure For water, wastewater, and seawater USEPA accepted for reporting wastewater analysis Enter the stored Press: Insert the COD/TNT Use a TenSette Pipet 82 ENTER program number for Adapter into the cell to add 5.0 mL of sample...
Page 364 PHOSPHORUS, REACTIVE, continued Clean the outside of Place the sample vial Tightly cover the Press: ZERO the vial with a towel. into the adapter. sample vial with the The cursor will move to instrument cap. Note: Wiping with a damp Push straight down on the right, then the towel, followed by a dry...
Page 365 PHOSPHORUS, REACTIVE, continued Tightly cover the Press: READ vial with the instrument The cursor will move to cap. the right, then the result in mg/L phosphate ) will be displayed. Note: Standard Adjust may be performed using a prepared standard (see Section 1).
Page 366 ±0.08 mg/L PO Estimated Detection Limit (EDL) The EDL for program 82 is 0.07 mg/L PO . For more information on derivation and use of Hach’s estimated detection limit, see Section 1.
Page 367 PHOSPHORUS, REACTIVE, continued Interferences The following may interfere when present in concentrations exceeding these listed below: Substance Interference Level and Treatment Aluminum 200 mg/L Arsenate Interferes at any level Chromium 100 mg/L Copper 10 mg/L Iron 100 mg/L Nickel 300 mg/L Silica 50 mg/L Silicate...
Page 368 PHOSPHORUS, REACTIVE, continued Summary of Method Orthophosphate reacts with molybdate in an acid medium to produce a phosphomolybdate complex. Ascorbic acid then reduces the complex, giving an intense molybdenum blue color. REQUIRED REAGENTS Reactive Phosphorus Test ’N Tube Reagent Set.........50 tests ..... 27425-45 Includes: (1) 21060-46, (50) Orthophosphate Dilution Vials* Quantity Required Description...
Page 369 Pipet Filler, Safety Bulb ................each....14651-00 Pipet, volumetric, Class A, 5.00 mL ............each....14515-37 Pipet, volumetric, Class A, 2.00 mL ............each....14515-36 For Technical Assistance, Price and Ordering In the U.S.A. call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 371: Phosphorus, Acid Hydrolyzable, Phosver 3 With Acid Hydrolysis
Method 8180 PHOSPHORUS, ACID HYDROLYZABLE (0.00 to 5.00 mg/L PO PhosVer 3 with Acid Hydrolysis For water, wastewater, and seawater Test ’N Tube Procedure ™ Turn on the COD Enter the stored Press: Insert the COD/TNT 82 ENTER Reactor. Heat to 150 °C. program number for acid Adapter into the cell The display will show...
Page 372 PHOSPHORUS, ACID HYDROLYZABLE, continued Clean the outside of Place the sample Tightly cover the vial Remove the cap the vial with a towel. vial in the adapter. with the instrument cap. from the vial. Using a funnel, add the contents Push straight down on Note: Wiping with a damp Press:...
Page 373 PHOSPHORUS, ACID HYDROLYZABLE, continued Tightly cover the Press: READ vial with the instrument The cursor will move to cap. the right, then the result in mg/L phosphate ) will be displayed. Note: Standard Adjust may be performed using a prepared standard (see Section 1).
Page 374 PHOSPHORUS, ACID HYDROLYZABLE, continued d) Analyze each sample as described in the procedure. Use 5.0 mL of the prepared standard additions for each test; the concentration should increase as follows: 0.2 mg/L, 0.4 mg/L, and 0.6 mg/L PO , respectively. e) If these increases do not occur, see Standard Additions in Section 1 for more information.
Page 375 PHOSPHORUS, ACID HYDROLYZABLE, continued Turbidity (large amounts) May cause inconsistent results because the acid present in the powder pillows may dissolve some of the suspended particles and because of variable desorption of orthophosphate from the particles. Zinc 80 mg/L Highly buffered samples or May exceed the buffering capacity of the reagents and extreme sample pH require sample pretreatment;...
Page 376 PHOSPHORUS, ACID HYDROLYZABLE, continued REQUIRED REAGENTS Total and Acid Hydrolyzable Test ’N Tube Reagent Set....... 50 tests..27427-45 Includes: (1) 272-42, (1) 1045-42, (1) 20847-66, (1) 21060-46, (50) Total and Acid Hydrolyzable Test Vials* (1) 27430-42 Quantity Required Description Per Test Unit Cat.
Page 377 Pipet, volumetric, Class A, 5.00 mL ............each....14515-37 Pipet, volumetric, Class A, 2.00 mL ............each....14515-36 Pipet Filler, safety bulb ................each....14651-00 For Technical Assistance, Price and Ordering In the U.S.A. call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 379: Phosphorus, Total, Phosver 3 With Acid Persulfate Digestion
Method 8190 PHOSPHORUS, TOTAL (0.00 to 3.50 mg/L PO For water, wastewater and seawater PhosVer 3 with Acid Persulfate Digestion USEPA Accepted for reporting wastewater analysis Test ’N Tube Procedure Turn on the DRB200 Enter the stored Press: Insert the COD/TNT 82 ENTER Reactor.
Page 380 PHOSPHORUS, TOTAL, continued Carefully remove the Use a TenSette Clean the outside of Place the sample vial from the reactor. Pipet to add 2.0 mL of the vial with a towel. vial in the adapter. Place it in a test tube 1.54 N sodium Push straight down on Note: Wiping with a damp...
Page 381 PHOSPHORUS, TOTAL, continued Press: After the timer Place the prepared Tightly cover the beeps, clean the outside sample vial in the vial with the instrument TIMER ENTER of the sample vial with adapter. cap. A 2-minute waiting a towel. Push straight down on period will begin.
Page 382 PHOSPHORUS, TOTAL, continued Sampling and Storage Collect samples in plastic or glass bottles that have been acid cleaned with 1:1 Hydrochloric Acid Solution and rinsed with deionized water. Do not use commercial detergents containing phosphates for cleaning glassware used in this test. Analyze samples immediately after collection for best results.
Page 383 PHOSPHORUS, TOTAL, continued acid-washed 100-mL Class A volumetric flask. Dilute to the mark with deionized water. Method Performance Precision In a single laboratory, using a standard solution of 3.00 mg/L and two lots of reagent with the instrument, a single operator obtained a standard deviation of ±0.06 mg/L PO Estimated Detection Limit The estimated detection limit for program 82 is 0.07 mg/L PO...
Page 384 PHOSPHORUS, TOTAL, continued Sample Disposal Information Final samples will contain molybdenum. In addition, final samples will have a pH less than 2 and are considered corrosive (D002) by the Federal RCRA. Summary of Method Phosphates present in organic and condensed inorganic forms (meta-, pyro- or other polyphosphates) must be converted to reactive orthophosphate before analysis.
Page 385 Pipet, TenSette, 0.1-1.0 mL..............each....19700-01 Pipet Tips, for 19700-01 TenSette Pipet ..........50/pkg....21856-96 Pipet Tips, for 19700-01 ..............1000/pkg....21856-28 For Technical Assistance, Price and Ordering In the U.S.A. call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 387: Phosphorus, Reactive, Amino Acid Method
Method 8178 PHOSPHORUS, REACTIVE (0 to 30.0 mg/L PO Amino Acid Method For water, wastewater, seawater Enter the stored Press: Fill a 25-mL sample Add 1 mL of 85 ENTER program number for cell with 25 mL of sample. Molybdate Reagent using The display will show reactive phosphate a 1-mL calibrated dropper.
Page 388 PHOSPHORUS, REACTIVE, continued Add 1 mL of Amino Press: Pour 25 mL of When the timer Acid Reagent Solution. sample (the blank) into a beeps, the display TIMER ENTER Cap and invert several sample cell. will show: A 10-minute reaction times to mix (the mg/L PO4 period will begin.
Page 389 PHOSPHORUS, REACTIVE, continued Analyze samples immediately for best results. If prompt analysis is not possible, preserve samples by filtering immediately and storing the sample at 4 °C (39 °F) for up to 48 hours. Accuracy Check Standard Additions Method a) Snap the neck off a Phosphate PourRite Ampule Standard Solution, 500 mg/L as PO b) Use the TenSette Pipet to add 0.1 mL, 0.2 mL and 0.3 mL of standard, respectively, to three 25-mL samples.
Page 390 PHOSPHORUS, REACTIVE, continued Interferences Interfering Substance Interference Levels and Treatments Calcium (Ca Greater than 10,000 mg/L as CaCO Chloride Greater than 150,000 mg/L as Cl Colored samples Add 1 mL of 10 N Sulfuric Acid Standard Solution to another 25-mL sample. Use this instead of untreated sample as the blank to zero the instrument.
Page 391 PHOSPHORUS, REACTIVE, continued Includes: (1) 1934-32, (1) 2236-32 Quantity Required Description Per Test Units Cat. No. Amino Acid Reagent ..........1 mL ..100 mL MDB ....1934-32 Molybdate Reagent ..........1 mL ..100 mL MDB* ....2236-32 REQUIRED APPARATUS Sample Cell, 10-20-25 mL, w/ cap .......2 ......6/pkg ..24019-06 OPTIONAL REAGENTS Description Units...
Page 392 Pipet Filler, safety bulb ................each ..12189-00 Spoon, measuring, 0.05 g ................each ....492-00 Thermometer, -20 to 110 °C, Non-Mercury ..........each..26357-02 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 393: Silica, Low Range Heteropoly Blue Method
Method 8186 SILICA, Low Range (0 to 1.60 mg/L) For water and seawater Heteropoly Blue Method Enter the stored Press: Fill two sample Add 15 drops of 90 ENTER program number for low cells to the 10-mL line Molybdate 3 Reagent to The display will show range silica (SiO with sample.
Page 394 SILICA, Low Range, continued The display will After the timer Press: Place the sample ZERO show: beeps, place the blank into the cell holder. The cursor will move to (solution without Amino Tightly cover the sample 2:00 TIMER 3 the right, then the Acid F Reagent) into the cell with the instrument display will show:...
Page 395 The estimated detection limit for program 90 is 0.020 mg/L SiO2. For more information on the estimated detection limit, see Section 1. If testing for very low levels of silica, use the ultra-low range silica method on the Hach DR/2010 or DR/4000 Spectrophotometers.
Page 396 SILICA, Low Range, continued Interferences Interfering Interference Levels and Treatments Substance Color Eliminated by zeroing the instrument with the original sample. Phosphate Phosphate does not interfere at levels less than 50 mg/L . At 60 mg/L PO , an interference of -2% occurs. At 75 mg/L PO the interference is -11%.
Page 397 Pipet Tips, for 19700-01 Pipet ............1000/pkg ..21856-28 Standard Methods for the Examination of Water and Wastewater....each ..22708-00 Thermometer, - 20 to 110 °C, Non-Mercury..........each ..26357-02 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 399: Silica, Ultra High Range Silicomolybdate Method
Method 10098 SILICA, Ultra High Range (0 to 200 mg/L) For water and seawater Silicomolybdate Method Enter the stored Press: Fill 2 sample cells Fill both sample cells 88 ENTER program number for with 10 mL of sample. to the 25-mL line with The display will show ultra high range silica deionized water.
Page 400 SILICA, Ultra High Range, continued The display will When the timer Press: Place the prepared ZERO show: 2:00 Timer 2 beeps, place the blank in sample into the cell The cursor will move to the cell holder. Tightly holder. Tightly cover the Press: the right, then the ENTER...
Page 401 SILICA, Ultra High Range, continued Sampling and Storage Collect samples in clean plastic or glass bottles. Analyze samples as soon as possible after collection. Store samples up to 28 days at ° C (39 ° F) or below. Warm samples to room temperature before analyzing.
Page 402 SILICA, Ultra High Range, continued Estimated Detection Limit The estimated detection limit for program 88 is 3.0 mg/L SiO For more information on the estimated detection limit, see Section 1. Interferences Interfering Substance Interference Levels and Treatments Color Eliminated by zeroing the instrument with the original sample.
Page 403 Pipet Filler, safety bulb ................each ..14651-00 Standard Methods for the Examination of Water and Wastewater.....each ..22708-00 Thermometer, -20 to 110 °C, Non-Mercury..........each ..26357-02 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 405: Sulfate, Sulfaver 4 Method
Method 8051 SULFATE (0 to 70 mg/L) For water, wastewater, and seawater SulfaVer 4 Method (Powder Pillows or AccuVac Ampuls); USEPA accepted for reporting wastewater analysis Using Powder Pillows Choose Desired Program Accuracy A User-Entered Enter the stored Press: Fill a clean sample 91 ENTER Calibration is necessary program number...
Page 406 SULFATE, continued Add the contents of Press: After the timer Place the blank into one SulfaVer 4 Sulfate beeps, fill a second the cell holder. Tightly TIMER ENTER Reagent Powder Pillow sample cell with 10 mL cover the sample cell A 5-minute reaction to the sample cell (the of sample (the blank).
Page 407 SULFATE, continued Using AccuVac Ampuls Choose Desired Program Accuracy A User-Entered Enter the stored Press: Fill a sample cell with 92 ENTER Calibration is necessary program number at least 10 mL of sample The display will show to obtain the most for sulfate (SO (the blank).
Page 408 SULFATE, continued Press: Within five minutes Press: ZERO READ after the timer beeps, The cursor will move to The cursor will move to place the AccuVac the right, then the the right, then the result ampul into the cell display will show: in mg/L sulfate will holder.
Page 409 SULFATE, continued Sampling and Storage Collect samples in clean plastic or glass bottles. Samples may be stored up to 28 days by cooling to 4 °C (39 °F) or lower. Warm to room temperature before analysis. Accuracy Check Standard Additions Method- Powder Pillows a) Snap the neck off a Sulfate Standard PourRite Ampule, 1000 mg/L SO b) Use a TenSette Pipet to add 0.1, 0.2 and 0.3 mL of...
Page 410 The EDL for program 91 is 4.9 mg/L SO and the EDL for program 92 is 3 mg/L SO . For more information on derivation and use of Hach’s estimated detection limit, see Section 1. Interferences The following interfere at levels above those concentrations listed:...
Page 411 Pipet, volumetric, 6.00 mL, Class A ............each ..14515-06 Pipet, volumetric, 7.00 mL, Class A ............each ..14515-07 Pipet Filler, safety bulb ................each ..14651-00 PourRite Ampule Breaker ................each ..24846-00 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 413: Sulfide, Methylene Blue Method
Method 8131 SULFIDE (0 to 0.70 mg/L S For water, wastewater and seawater Methylene Blue Method USEPA accepted for reporting wastewater analysis Enter the stored Press: Pipet 25 mL of Fill a second sample 93 ENTER program number for sample into a clean cell with 25 mL of The display will show sulfide (S).
Page 414 ± 0.02 mg/L sulfide. Estimated Detection Limit (EDL) The EDL for program 93 is 0.01 mg/L S . For more information on derivation and use of Hach’s estimated detection limit, see Section 1.
Page 415 SULFIDE, continued Interferences Interfering Interference Levels and Treatments Substance Strong reducing Interfere by reducing the blue color or preventing substances (sulfite, its development. thiosulfate and hydrosulfite) Sulfide, high levels High concentrations of sulfide may inhibit full color development and require sample dilution. Some sulfide loss may occur when the sample is diluted.
Page 416 Dropper, for 1 oz. bottle................each.... 2258-00 Flask, erlenmeyer, 50 mL ................each....505-41 Standard Methods for the Examination of Water and Wastewater ..... each..22708-00 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 417: Surfactants, Anionic (Also Called: Detergents) Crystal Violet Method
Method 8028 SURFACTANTS, ANIONIC (0 to 0.300 mg/L) For water, wastewater, and seawater (Also called: Detergents) Crystal Violet Method Enter the stored Press: Fill a clean 500-mL Add 10 mL of 26 ENTER program number for graduated cylinder to the Sulfate Buffer Solution.
Page 418 SURFACTANTS, ANIONIC, continued After the timer Drain the top Fill another sample Place the blank in beeps, remove the benzene layer into a cell to the 25-mL mark the cell holder. Tightly stopper and drain the clean sample cell (the with pure benzene cover the sample cell bottom water layer.
Page 419 SURFACTANTS, ANIONIC, continued Sampling and Storage Collect samples in clean plastic or glass bottles. Analyze samples as soon as possible, but they may be stored at least 24 hours by cooling to 4 °C (39 °F). Warm to room temperature before testing. Accuracy Check Standard Additions Method a) Snap the neck off a Detergent Voluette Ampule Standard...
Page 420 Pipet Tips, for 19700-01 Pipet ..............50/pkg..21856-96 Pipet Tips, for 19700-01 Pipet ............1000/pkg..21856-28 Thermometer, -20 to 110 °C, Non-Mercury ..........each..26357-02 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 421: Suspended Solids Photometric Method
Method 8006 SUSPENDED SOLIDS (0 to 750 mg/L) For water and wastewater Photometric Method (Also called Nonfilterable Residue) 2:00 Enter the stored Press: Blend 500 mL of Pour the blended 94 ENTER program number for sample in a blender sample into a The display will show suspended solids.
Page 422 In a single laboratory, using a standard solution of 847.4 mg/L Suspended Solids with the instrument, a single operator obtained a standard deviation of ±18.2 mg/L Suspended Solids. For more information on Hach’s precision statement, see Section 1. Estimated Detection Limit The estimated detection limit for program 94 is 22.1 mg/L...
Page 423 Pipet, Filler, safety bulb ..........1 ......each ..14651-00 OPTIONAL APPARATUS Stirring Rod, glass ..................3/pkg ... 1770-01 Wash Bottle, 250 mL...................each ....620-31 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 425: Tannin And Lignin Tyrosine Method
Method 8193 TANNIN AND LIGNIN (0 to 9.0 mg/L) For water, wastewater, boiler water Tyrosine Method Enter the stored Press: Fill a clean sample Fill a clean sample 98 ENTER program number for cell to the 25-mL mark cell to the 25-mL mark The display will show tannin and lignin.
Page 426 TANNIN AND LIGNIN, continued Press: Place the prepared Press: ZERO READ sample into the cell The cursor will move to The cursor will move to holder. Tightly cover the the right, then the the right, then the result sample cell with the display will show: in mg/L tannic acid will instrument cap.
Page 427 TANNIN AND LIGNIN, continued Interferences Substance Interference Level and Treatment Ferrous iron Causes a positive interference. Two mg/L of ferrous iron produces a color equivalent to about 1 mg/L of tannic acid. To eliminate interference of ferrous iron up to 20 mg/L, add one 0.2-g scoop of sodium pyrophosphate to the sample before testing.
Page 428 Pipet, Filler, safety bulb ................each..14651-00 Spoon, measuring, 0.2 g................each....638-00 Weighing Boat, 67/47 mm ..............500/pkg..21790-00 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 429: Toxtrak
Method 10017 TOXTRAK TOXICITY TEST ™ For water and wastewater Colorimetric Method Inoculum Development Using Indigenous Biomass Incubate at 37 °C until the vial contents Using one of the are visibly turbid dropper pipets provided, (turbidity indicates add 1.0 mL of source bacterial growth).
Page 430 TOXTRAK TOXICITY TEST, continued Colorimetric Reaction Enter the stored Press: Insert the TNT/COD Fill a Test ‘N Tube 61 ENTER program number Adapter into the cell vial with deionized The display will show: for toxicity. holder by rotating the water. Label this vial as ABS 610 nm adapter until it drops the “blank”.
Page 431 TOXTRAK TOXICITY TEST, continued Add 5.0 mL of Add 5.0 mL of the Add 2 drops of Add 0.5 mL of deionized water to the sample (or dilution) to Accelerator Solution to inoculum (previously control tube. each sample vial. each vial. Cap and invert prepared) to each vial.
Page 432 TOXTRAK TOXICITY TEST, continued After the absorbance Press: Place the “control” Place each sample ZERO of the “control” vial has vial in the cell holder. or dilution vial in the The cursor will move to decreased 0.60 ±0.10 Tightly cover the vial cell holder.
Page 433 TOXTRAK TOXICITY TEST, continued Interpreting Results The Percent Inhibition results obtained are only a relative measurement. They do not represent a true quantitative measurement of toxic concentration. The Percent Inhibition does not necessarily increase in direct proportion to the concentration of toxins.
Page 434 TOXTRAK TOXICITY TEST, continued laundry bleach. Pour the test container contents and test containers into the bleach solution. Allow 10-15 minutes of contact time with the bleach solution. Then pour the liquid down the drain and wash the reaction tubes for re-use. Summary of Method Resazurin is a redox-active dye, which changes from pink to blue when it is reduced.
Page 435 Incubator, 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 Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 437: Turbidity Absorptometric Method
Method 8237 TURBIDITY (0 to 1000 FAU) For water, wastewater, and seawater Absorptometric Method 95 ENTER Enter the stored Press: Fill a sample cell Place the blank into program number for The display will show with 10 mL of deionized the cell holder.
Page 438 2. Dilute to the mark with deionized water. Prepare this daily. Convenient stabilized turbidity stock solution (200 NTU ™ StablCal Standard) is available from Hach. Standard Adjust To adjust the calibration curve using the reading obtained with 200 FAU formazin standard, press the...
Page 439 TURBIDITY, continued Interferences Interfering Substance Interference Levels and Treatments Air Bubbles Interfere at all levels. Degass samples using the Degassing Kit or an ultrasonic bath. Color Interferes if the color absorbs light at 520 nm. Temperature extremes May interfere by changing the turbidity of the sample. Analyze samples as soon as possible after collection.
Page 440 Stopper, rubber, one-hole, No. 7 ............... 6/pkg.... 2119-07 Tubing, rubber, 5/16” I.D................ 12 feet....560-19 Tweezers, plastic ..................each..14282-00 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 441: Volatile Acids Esterification Method
TenSette Pipet. dissolved solids or mineral The display will show: acids are present, distill as Note: Adjust the pH of PRGM ? described in the Hach stored samples before Distillation Apparatus analysis. Note: For most accurate manual. results, perform a Reagent...
Page 442 VOLATILE ACIDS, continued Press: When the timer Pipet 0.5 mL of Pipet 2.0 mL of TIMER beeps, cool solutions to Hydroxylamine 4.5 N Sodium ENTER 25 °C (until cells feel Hydrochloride Solution Hydroxide Standard A 3-minute reaction cool) with running tap into each cell.
Page 443 VOLATILE ACIDS, continued Press: Place the prepared Press: ZERO READ sample into the cell The cursor will move to The cursor will move to holder. Tightly cover the the right, then the the right, then the result sample cell with the display will show: in mg/L Volatile Acids instrument cap.
Page 444 VOLATILE ACIDS, continued Standard Solution Method Prepare a 500 mg/L volatile acid standard by using the TenSette Pipet to add 0.8 mL of a Volatile Acids PourRite Ampule Standard Solution (62,500 mg/L as acetic acid) to a 100-mL volumetric flask. Dilute to volume with deionized water. Stopper and invert to mix.
Page 445 Pipet Tips, for 19700-01 TenSette Pipet ..........1000/pkg ..21856-28 Pipet, TenSette, 1.0 to 10.0 mL ..............each ..19700-10 Pipet Tips, for 19700-10................50/pkg ..21997-96 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 447: Zinc, Zincon Method
Method 8009 ZINC (0 to 3.00 mg/L Zn) For water and wastewater * USEPA approved for wastewater analysis Zincon Method (digestion needed; see Section 2) Enter the stored Press: Fill a 25-mL sample Add the contents of 97 ENTER program number cell with 20 mL one ZincoVer 5 Reagent The display will show...
Page 448 ZINC, continued Measure 10 mL of Add 0.5 mL of Tightly cap the cell. Press: the orange solution into cyclohexanone to the Shake vigorously for 30 TIMER ENTER another sample cell remaining orange seconds (the prepared A 3-minute reaction (the blank). solution in the first sample).
Page 449 ±0.02 mg/L Zn. Estimated Detection Limit (EDL) The EDL for program 97 is 0.02 mg/L Zn. For more information on derivation and use of Hach’s estimated detection limit, see Section 1.
Page 450 ZINC, continued Interferences The following may interfere when present in concentrations exceeding those listed below. Interfering Substance Interference Level and Treatments Aluminum 6 mg/L Cadmium 0.5 mg/L Copper 5 mg/L Iron (ferric) 7 mg/L Manganese 5 mg/L Nickel 5 mg/L Organic material Large amounts may interfere.
Page 451 ZINC, continued Summary of Method Zinc and other metals in the sample complex with cyanide. Adding cyclohexanone selectively releases zinc. The zinc then reacts with the 2-carboxy-2’-hydroxy-5’-sulfoforamazyl benzene (zincon) indicator and forms a blue color that is proportional to the zinc concentration.
Page 452 Pipet, TenSette, tips for 19700-10 ............250/pkg..21997-25 Pipet, volumetric, Class A, 5.00 mL............each..14515-37 Pipet, volumetric, Class A, 0.5 mL............. each..14515-34 For Technical Assistance, Price and Ordering In the U.S.A.—Call 800-227-4224 Outside the U.S.A.—Contact the Hach office or distributor serving you.
Page 453: How To Order
Quantity Technical and Customer Service Hach Technical and Customer Service Department personnel are eager to answer questions about our products and their use and to take your orders. Specialists in analytical methods, they are happy to put their talents to...
Page 454 Customers may send remittance with orders or we can ship C.O.D. if you prefer. Warranty Hach warrants its products to be of high quality, to be free of material defects on the date of shipment and to be as specified. Limits of Usage Our chemicals and reagents are offered for laboratory and manufacturing use ONLY.
Page 455: Additional Information
Product Name -- In French, German, Italian and Spanish as well as English is printed on all but the smallest-size labels. • Hach Catalog Number -- Makes reordering easy and helps match the appropriate MSDS. • Storage Information and Lot Numbers -- Lot numbers made up of letters and numbers indicate an extended shelf life;...
Page 457 ADDRESS A one- or two-word CITY STATE description of the item. ATTENTION If more than one size HACH ACCOUNT NO. (If available) of an item is offered, PAYMENT METHOD: Check MasterCard Visa Purchase Order state the size you want.
Page 458 UNIT UNIT QUANTIT CAT. NO. DESCRIPTION SIZE PRICE TOTAL Shipping Charge Prices are subject to change without notice TAXABLE? *If no, tax exempt document is: Enclosed On file at Hach TOTAL ORDER...

Hach DR/850 Procedures Manual

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