Page 3
Table of Contents Hach Company Trademarks ........................2 Section 1 Introduction ........................13 1.1 Abbreviations Used in this Manual ........................13 1.2 Conversions................................14 1.2.1 Chemical Species............................14 1.2.2 Hardness...............................14 Section 2 Laboratory Practices ......................15 2.1 Temperature ................................15 2.2 Mixing ..................................15 2.3 Digestion ................................15 2.3.1 EPA Mild Digestion with Hot Plate for Metals Analysis Only ............16 2.3.2 EPA Vigorous Digestion with Hot Plate for Metals Analysis Only.............16...
Page 4
Table of Contents 3.4.2 Method Detection Limit (MDL) ........................42 3.4.3 Precision ...............................44 3.4.4 Estimating Precision ...........................44 3.4.5 Sensitivity..............................44 3.5 Preparing a Calibration Curve..........................45 3.5.1 %T Versus Concentration Calibration......................45 3.5.2 Absorbance Versus Concentration Calibration..................47 3.6 Adapting Procedures to Other Spectrophotometers ..................47 3.6.1 Selecting the Best Wavelength........................47 3.7 Comparison of International Drinking Water Guidelines................52 3.7.1 Definitions of USEPA Approved and Accepted..................53...
Page 5
Table of Contents (Denotes USEPA accepted or approved for water or wastewater analysis. 4.7.1 How to Obtain an MSDS..........................60 4.7.2 Sections of an MSDS ...........................61 4.7.3 OSHA Chemical Hygiene Plan .........................62 Section 5 Procedures Explained ......................63 Alachlor Immunoassay Method Aluminum Method 8012 Aluminon Method Powder Pillows...
Page 6
Table of Contents (Denotes USEPA accepted or approved for water or wastewater analysis. Chlorine Dioxide Amaranth Method (20 to 500 µg/L) Chlorine Dioxide Method 8065 Chlorophenol Red Method LR (0.01 to 1.00 mg/L) ✭Method 8021 Chlorine, Free DPD Method ® Powder Pillows or AccuVac Ampuls (0.02 to 2.00 mg/L)
Page 7
Table of Contents (Denotes USEPA accepted or approved for water or wastewater analysis. Copper Bathocuproine Method UniCell™ Vials (0.10 to 6.00 mg/L) Cyanide Method 8027 Pyridine-Pyrazalone Method – Powder Pillows (0.001 to 0.240 mg/L CN Cyanide Cyanogen Chloride – UniCell™ Vials (0.01 to 0.50 mg/L CN Cyanuric Acid Method 8139...
Page 8
Table of Contents (Denotes USEPA accepted or approved for water or wastewater analysis. Lead PAR Method UniCell™ Vials (0.20 to 2.00 mg/L) ✭Method 8034 Manganese Periodate Oxidation Method Powder Pillows HR (0.2 to 20.0 mg/L) Manganese Method 8149 1-(2-Pyridylazo)-2-Naphthol PAN Method Powder Pillows LR (0.007 to 0.700 mg/L) Mercury...
Page 9
Table of Contents (Denotes USEPA accepted or approved for water or wastewater analysis. Powder Pillows (0.01 to 0.50 mg/L NH –N) Nitrogen, Ammonia Method 10031 Salicylate Method ™ Test ‘N Tube Vials HR (0.4 to 50.0 mg/L NH –N) Nitrogen, Ammonia Method 10023 Salicylate Method Test ‘N Tube™...
Page 10
Table of Contents (Denotes USEPA accepted or approved for water or wastewater analysis. 3 to 450 µg/L DEHA; 9 to 1000 µg/L hydroquinone; 13 to 1500 µg/L iso-ascorbic acid [ISA]; 15 to 1000 µg/L methylethyl ketoxime [MEKO] Ozone Method 8311 Indigo Method ®...
Page 11
Table of Contents (Denotes USEPA accepted or approved for water or wastewater analysis. 3– Test ‘N Tube™ Vials HR (1.0 to 100.0 mg/L PO Phosphorus, Total Ascorbic Acid Method with Acid Persulfate Digestion 3– UniCell™ Vials (1.5 to 15.0 mg/L PO Phosphorus, Total Ascorbic Acid Method with Acid Persulfate Digestion 3–...
Page 12
Volatile Acids Method 8196 Esterification Method (27 to 2800 mg/L) ✭Method 8009 Zinc Zincon Method Powder Pillows (0.01 to 2.00 mg/L) Zinc UniCell™ Vials (0.10 to 6.00 mg/L Zn) Table of Contents Page 12 5940022TOC.fm...
(ppb) Standard Federation (WEF), is the standard reference Methods work for water analysis. Order from Hach milliliter—1/1000 of a liter. It is approximately requesting Cat. No. 22708-00, or from the the same as a cubic centimeter (and is Publication Office of the APHA.
Page 14
Introduction 1.2 Conversions 1.2.1 Chemical Species 1.2.2 Hardness Table 2 lists the factors for converting hardness from one unit of measure to another. 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 American...
Page 15
Section 2 Laboratory Practices 2.1 Temperature Most tests in this manual perform most accurately when the sample temperature is between 20 °C and 25 °C (68 to 77 °F). A note in the individual procedure will state any special temperature requirements. 2.2 Mixing Swirling is recommended when mixing samples in a graduated cylinder or a titration flask.
Page 16
Laboratory Practices The Hach Digesdahl system is a process that yields a digest suitable for the determination of metals, total phosphorus and total Kjeldahl nitrogen (TKN). It is rapid, convenient, and the method of choice. For USEPA reporting purposes, USEPA-approved digestions are required.
Page 17
Heater and Support Apparatus, which comes in a 115 VAC, 60 Hz model (Cat. No. 22744-00) and a 230 VAC, 50 Hz model (Cat. No. 22744-02). The Hach Distillation Apparatus is suitable for water and wastewater that requires sample pretreatment by distillation. Applications for the General Purpose Apparatus include: fluoride, albuminoid nitrogen, ammonia nitrogen, phenols, selenium, and volatile acids.
Page 18
Laboratory Practices Figure 2 General Purpose Distillation Apparatus 2.5 Filtration Filtration separates particulates from an aqueous sample. It uses a porous medium that retains particulates but allows liquids to pass through. It is useful for removing turbidity (which may interfere in colorimetric analyses) from water samples.
Page 20
In some cases, reaction with the storage container or interaction of reagent components may occur. In its quest for reagent stability, Hach has developed many unique formulations, methods of analysis, and forms of packaging.
Page 21
It is then best to use a reagent blank prepared as above. 2.7 Sample Dilution Most Hach colorimetric tests use volumes of 10 and 25 mL. However, in some tests, the color developed in the sample may be too intense to be measured due to high levels of analyte, or unexpected colors may develop due to an interference.
Page 22
Laboratory Practices More accurate dilutions can be done with a pipet and a 100-mL volumetric flask (see Table 5 for more information). Pipet the sample and dilute to volume with deionized water. Swirl to mix. Table 5 Multiplication Factors for Diluting to 100 mL Sample Volume (mL) Multiplication Factor 2.7.1 Sample Dilution with Interfering Substances...
Page 23
Laboratory Practices 3. Invert the ampule several times to dissolve the reagent. Do not place your finger over the broken end; the liquid will stay in the ampule when inverted. Wipe the ampule with a lint-free cloth to remove fingerprints, etc. 4.
Page 24
Laboratory Practices 2.10.3 Cleaning of Sample Cells Most laboratory detergents can be used at recommended concentrations. Neutral detergents, such as Liquinox, are safer when regular cleaning is required. When using a detergent, you can clean faster by increasing the temperature, or by using an ultrasonic bath. Finish by rinsing a few times with deionized water and allow to air dry.
Page 25
See your Instrument Manual for instructions on installation. Not all procedures allow for using the Cell. The Pour-Thru Cell can be used with Hach chemistries provided a 25 mL sample is analyzed. Exceptions are noted in Table 6.
Page 26
If the windows appear hazy, soak the cell in a detergent bath and rinse thoroughly with deionized water. Note: The Cell cannot be used directly with Hach programs unless it is specified in the procedure. Using the Pour-Thru Cell with other Hach procedures requires a standard adjust or entering a dilution factor of 0.95.
Page 27
Section 3 Chemical Analysis 3.1 Sample Collection, Preservation, and Storage Correct sampling and storage are critical for accurate testing. Sampling devices and containers must be thoroughly clean to prevent carryover from previous samples. Preserve the sample properly; each procedure has information about sample preservation.
Page 28
Chemical Analysis d. Rinse well with deionized water. For chromium, 12–15 rinses may be necessary. When determining ammonia and Kjeldahl nitrogen, the rinse water must be ammonia-free. e. Air dry. Protect the glassware from fumes and other sources of contamination when storing. Use chromic acid or chromium-free substitutes to remove organic deposits from glass containers.
Page 29
1000 × 10.0 mg/L 1.007 10.07 mg/L correct result Hach 1:1 Nitric Acid Pillows contain 2.5 mL of acid: correct for this volume. Table 8 Required Containers, Preservation Techniques and Holding Times Maximum Holding Parameter No./Name Container Preservation Time Table 1A - Bacterial Tests 1–4.
Page 30
Chemical Analysis Table 8 Required Containers, Preservation Techniques and Holding Times (continued) Maximum Holding Parameter No./Name Container Preservation Time 27. Hardness P, G to pH<2, H to pH<2 6 months 28. Hydrogen ion (pH) P, G None required Analyze immediately 31, 43.
Page 31
Chemical Analysis Polyethylene (P) or glass (G), or PTFE Teflon Sample preservation should be performed immediately upon sample collection. For composite chemical samples each portion should be preserved at the time of collection. When use of an automated sampler makes it impossible to preserve each portion, then chemical samples may be preserved by maintaining at 4 °C until compositing and sample splitting is completed.
Page 32
Chemical Analysis 3.2.2 Standard Additions In general, this technique requires adding a small amount of a standard solution to the sample water and repeating the procedure. You should get close to 100% recovery. If not, a problem exists and must be identified. 1.
Page 33
Chemical Analysis Figure 9 Standard Additions Decision Tree Did a Single Standard Addition Give the Correct Recovery? Interferences Interferences Present? Present? Do Multiple Analysis Standard Additions Is Correct On DI Water Give Correct Recovery? Is the Procedure in Do Multiple Standard Use Correct? Additions On Sample Give Uniform Increments?
Page 34
Chemical Analysis mL standard added mg/L standard added mg/L analyte found These data show several points: • The standard added to the deionized water was completely recovered. Therefore, the chemicals, instrument, procedure/technique, and standards are working correctly. • The standard added to the original sample was not completely recovered; therefore, the sample contains an interference.
Page 35
Chemical Analysis Example A mL standard added mg/L standard added mg/L analyte found 1.10 1.18 1.23 Example B mL standard added mg/L standard added mg/L analyte found Figure 10 Multiple Standard Additions — A and B mg/L ACTUALLY PRESENT mg/L STANDARD ADDED The plot for Example A illustrates an interference that becomes progressively worse as the concentration of the standard or analyte increases.
Page 36
Chemical Analysis Example C mL standard added mg/L standard added mg/L analyte found Example D mL standard added mg/L standard added mg/L analyte found Figure 11 Multiple Standard Additions — C and D mg/L ACTUALLY PRESENT mg/L STANDARD ADDED The plot for Example C illustrates a common interference with a uniform effect on the standard and the substances in the sample.
Page 37
1-800-227-4224 or visit our Web site: http://www.hach.com/forms.htm. Troubleshooting a Test When Results are in Doubt If the results from any Hach chemistry are in doubt, troubleshoot them as follows: 1. Run a proof-of-accuracy check. Take a standard solution, which has a known concentration, through the same steps as the original sample.
Page 38
3. If the standard solution check does not match the expected results, check the reagents used in the test and the analytical technique as follows: a. Determine the age of the reagents used in the test. While most Hach reagents have a long shelf life, many factors affect this (i.e., storage temperature, storage conditions, microbial contamination).
Page 39
Chemical Analysis Because it may not be feasible to determine the cause of the interference, diluting the sample past the point of interference is often the most economical and efficient means of getting the correct result. If it is not possible to dilute out an interference without diluting out the parameter to be measured, use a different method, such as a different chemistry or an ion-selective electrode to measure the parameter.
Page 40
The instrument will remember the factor until the program is exited and will display the standard adjustment icon when it is used. You can return to the pre-programmed curve any time by selecting the Hach Program from the main menu.
Page 41
“General Introduction.” pH Interference Chemical reactions are often pH dependent. Hach reagents contain buffers to adjust the pH of the sample to the correct range. However, the reagent buffer may not be strong enough for samples that are highly buffered or have an extreme pH.
Page 42
MDL does not account for variation in sample composition and can only be achieved under ideal conditions. 1. Estimate the detection limit. Use the Hach sensitivity value stated in the Method Performance section of the analysis procedure. 2. Prepare a laboratory standard of the analyte, 1 to 5 times the estimated detection limit, in deionized water that is free of the analyte.
Page 43
MDL for FerroZine method = 2.998 (Student’s t ) x 0.0009 (s) MDL = 0.003 mg/L (agrees with initial estimate) 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.
Page 44
Some newer procedures use a 95% or 99% confidence interval, which is based on the calibration data for that particular chemistry. In replicate analysis, a Hach chemist prepares a specific concentration of the analyte in a deionized water matrix. The standard is then analyzed seven individual times on a single instrument with the two reagent lots originally used in the calibration (a total of 14 samples).
Page 45
Chemical Analysis Use sensitivity when comparing different methods. For example, Hach has three DR/2400 methods for determining iron: Iron Analysis ∆Abs ∆Concentration Portion of Curve Method FerroVer Entire range 0.010 0.022 mg/L FerroZine Entire range 0.010 0.009 mg/L TPTZ Entire range 0.010...
Page 46
Chemical Analysis Figure 12 Semilogarithmic Calibration Curve mg/L IRON To convert %T readings to concentration, prepare a table such as Table 9 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 % transmittance reading and the %T Units value is the second number of the % transmittance reading.
Page 47
Regardless of the spectrophotometer used, prepare the sample and calibration standards following the Hach procedure and use the optimum wavelength used in the Hach procedure. To calibrate for a given analyte, a series of standards are prepared and measured to establish the calibration curve.
Page 48
Chemical Analysis Table 10 Wavelength Absorbance 550 nm 0.477 500 nm 0.762 450 nm 0.355 400 nm 0.134 9. Adjust the wavelength to 50 nm more than the highest absorbance point on the initial search (step 8). Re-zero as in step 5. 10.
Page 49
Chemical Analysis Figure 13 Selecting the Best Wavelength 500 505 510 515 520 Wavelength (nm) Adapting a Buret Titration for Use With a Digital Titrator Any standard titration procedure that uses a buret can be adapted to the Digital Titrator by using the following procedure. 1.
Page 50
Chemical Analysis 3. When using the Digital Titrator for your buret method, note the number of digits required for a sample titration. To convert the digits required to the equivalent number of milliliters for a buret method, calculate: × --------------------- - Equivalent Buret Milliliters Digits Required ×...
Page 51
Chemical Analysis Table 12 (continued) Description Cat. No. PAO, phenylarsine oxide, 0.0451 N 21420-01 Potassium Dichromate, 1.00 N 21971-01 Silver Nitrate, 0.2256 N 14396-01 Silver Nitrate, 1.128 N 14397-01 Sodium Hydroxide, 0.1600 N 14377-01 Sodium Hydroxide, 0.1612 N 24280-02 Sodium Hydroxide, 0.3636 N 14378-01 Sodium Hydroxide, 0.9274 N 14842-01...
Page 52
Chemical Analysis 3.7 Comparison of International Drinking Water Guidelines Table 13 Comparison of International Drinking Water and FDA Bottled Water Guidelines Bottled Water USEPA Canada Japan U.S. Federal Maximum Maximum Maximum Maximum Parameter Drug Contaminant Acceptable Admissible Admissible Guideline Administration Level (MCL) Concentration Concentration...
Page 53
Chemical Analysis Table 13 Comparison of International Drinking Water and FDA Bottled Water Guidelines (continued) Bottled Water USEPA Canada Japan U.S. Federal Maximum Maximum Maximum Maximum Parameter Drug Contaminant Acceptable Admissible Admissible Guideline Administration Level (MCL) Concentration Concentration Concentration Level 6.5–8.5 6.5–8.5 6.5–9.5...
Page 54
Regulations. USEPA-approved methods may be used for reporting results to the 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. These methods are not published in the Federal Register, but are referenced to the equivalent USEPA method in the procedure.
Page 55
Section 4 Waste Management and Safety This section provides guidelines for laboratory waste management. These guidelines are only a summary of basic USEPA requirements, and do not relieve the user from complying with the complete regulations contained in the Code of Federal Regulations (CFR).
Page 56
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 261.20 through 40 CFR 261.33.
Page 57
For more information on using the MSDS, see Material Safety Data Sheets on page 60. Some Hach tests use or produce a number of chemicals that make the end product a hazardous waste; for example, the COD tests and Nessler’s reagent.
Page 58
Waste Management and Safety 4.4 Management of Specific Wastes Hach has several documents to assist customers in managing waste that has been generated from our products. You can obtain the following documents by calling 1-800-227-4224 or 970-669-3050 and requesting the literature codes given:...
Page 59
Waste Management and Safety 3. Task Force on Laboratory Waste Management. Less is Better; 2nd ed.; American Chemical Society, Department of Government Relations and Science Policy: Washington, DC 1993. 4. Committee on Chemical Safety. Safety in Academic Chemistry Laboratories, 5th ed.;...
Page 60
This section explains the information found on a Hach MSDS, and tells 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.
Page 61
Each MSDS has ten sections. The sections and the information found in them are described below. Header Information The Hach catalog number, MSDS date, change number, company address and telephone number, and emergency telephone numbers are listed at the top of the MSDS.
Page 62
Waste Management and Safety • Lower Flammable Limit (LFL or LEL): The lowest concentration that will produce a fire or flash when an ignition source is present. • Upper Flammable Limit (UFL or UEL): The vapor concentration in air above which the concentration is too rich to burn.
Page 63
• Sulfide 2 reagent contains potassium dichromate. The final solution will contain hexavalent chromium (D007) at a concentration regulated as a hazardous waste by Federal RCRA. Please see Section 4 for further information on proper disposal of these materials. Instrument Method 8131 display Hach Programs Procedure 25 mL 25 mL 25 mL 25 mL...
Page 64
Procedures Explained Levels of common sample substances or conditions that will Confirm cause inaccurate accuracy with results these steps (in addition, may also be used to Sulfide troubleshoot a Interferences test, improve technique, Interfering Substance Interference Levels and Treatments check Strong reducing substances Interfere by reducing the blue color or preventing its development (sulfite, thiosulfate and hydrosulfite)
Page 65
• Twenty Antibody Cuvettes are provided with each reagent set. One Antibody Cuvette will be used for each calibrator and each sample. Cuvettes are not reusable. Note: Hach Company recommends wearing protective nitrile gloves for this procedure. Alachlor Page 1 of 8...
Page 66
Alachlor Immunoassay Procedure for Water λ Touch Label an Antibody Place the cuvettes Pipet 0.5 mL of each Cuvette for each into the rack snugly. calibrator into the Single Wavelength calibrator and each appropriately labeled λ then touch the button. sample to be tested.
Page 67
Alachlor At the end of the Wash each cuvette 20-minute period, discard forcefully and thoroughly the contents of all the four times with deionized cuvettes into an water. Empty the rinse appropriate waste water into the waste container. container. Note: Ensure that most of the water is drained from the cuvettes by turning the cuvettes upside down and tapping them...
Page 68
Alachlor Measuring the Color Zero Label and fill a Install the 1-cm Touch Place the first Zero Zeroing Cuvette with square cell adapter. calibrator into the cell The display will show: deionized water. Wipe adapter. Note: See Section 2.6 Sample 0.000 Abs the outside of all the Cell Adapters in the Instrument...
Page 69
Alachlor Using the 1-cm MicroCuvette Rack This rack (see Figure 14) has been designed specifically to aid in achieving precise and accurate results when using the immunoassay technique to analyze several samples at the same time. Figure 14 The 1-cm MicroCuvette Rack Loading the Rack —...
Page 70
Alachlor Interpretation Sample #1 — Sample reading is less than the readings for both calibrators. Therefore the sample concentration of Alachlor is greater than both 0.1 ppb and 0.5 ppb Alachlor. Sample #2 — Sample reading is between the readings for the 0.1 ppb and 0.5 ppb Alachlor calibrators.
Page 71
2 ppb. Summary of Method Hach immunoassay tests use antigen/antibody reactions to test for specific organic compounds in water and soil. Alachlor-specific antibodies, attached to the walls of plastic cuvettes, selectively bind and remove Alachlor from complex sample matrices.
Page 72
Wipes, disposable ....................... box .....20970-00 ® TenSette , Pipet, 0.1–1.0 mL....................each....19700-01 Tips, for pipettor 19700-01....................1000/pkg...21856-28 * Immunoassay components are manufactured for Hach Company by Beacon Analytical Systems, Inc. FOR TECHNICAL ASSISTANCE, PRICE INFORMATION AND ORDERING: HACH COMPANY In the U.S.A. – Call...
Page 73
• Clean the graduated cylinder and sample cells with soap and a brush immediately following the test. Powder Pillows Method 8012 Hach Programs Touch Fill the cylinder to the Add the contents of Add the contents of 50-mL mark with sample.
Page 74
Aluminum 25 mL 20 mL 10 mL Touch the timer icon. Pour 25 mL of the Add the contents of Touch the timer icon. mixture into a 25-mL one Bleaching 3 Reagent Touch Touch sample cell. (This is the Powder Pillow to the Invert repeatedly for one Vigorously shake for 30 prepared sample.)
Page 75
Aluminum Interferences Interfering Substance Interference Levels and Treatments Greater than 300 mg/L as CaCO . Samples with greater than 300 mg/L acidity as CaCO must be treated as follows: a) Add one drop of m-Nitrophenol Indicator Solution (Cat. No. 2476-32) to the sample taken in step 3.
Page 76
Aluminum Figure 1 Fluoride Interference Graph mg/L Al (Reading from instrument) True Aluminum Concentration Sample Collection, Storage and Preservation Collect samples in a clean glass or plastic containers. Preserve the sample by adjusting the pH to 2 or less with nitric acid (Cat. No. 152-49) (about 1.5 mL per liter).
Page 77
Aluminum Standard Solution Method 1. Prepare a 0.4-mg/L aluminum standard solution as follows: Pipet 1.00 mL of Aluminum Standard Solution, 100-mg/L as Al , into a 250-mL volumetric flask. 2. Dilute to the mark with deionized water. Prepare this solution daily. Perform the aluminum procedure as described above.
Page 79
• Wipe the outside of sample cells before each insertion into the instrument cell holder. Use a damp towel followed by a dry one to remove fingerprints or other marks. Powder Pillows Method 8326 Hach Programs Touch Fill a 25-mL Add the contents of...
Page 80
Aluminum Touch the timer icon. After 30 seconds add Stopper and invert to Put one drop of ECR the contents of one mix until the powder is Masking Reagent Touch Hexamethylene- dissolved. Solution into a clean, A 30-second reaction tetramine Buffer Reagent round sample cell.
Page 81
Aluminum Zero Read 10 mL Touch Immediately wipe the Touch Zero Read prepared sample and The display will show: Results will appear in place it into the cell mg/L Al 0.008 mg/L Al holder. This test uses a non-zero intercept for the calibration curve.
Page 82
Aluminum a. Rinse a 50-mL graduated mixing cylinder and a 125-mL Erlenmeyer flask containing a magnetic stir bar with 6 N hydrochloric acid (Cat. No. 884-49). Rinse again with deionized water. This will remove any aluminum present. Note: Rinse two Erlenmeyer flasks if a reagent blank is used; see step b below. b.
Page 85
• Underrange appears on the display when the instrument is zeroed or when the determined sample concentration is below the operating range listed for this method. UniCell Vials Hach Programs Touch Pipet 2 mL of Buffer Pipet 3 mL of sample...
Page 86
Aluminum Zero Cap the vial. Invert Touch the timer icon. Install the 16-mm cell Touch Zero the sample until the adapter. Touch The display will show: solids dissolve Note: See Section 2.6 Sample A 25-minute reaction 0.00 mg/L Al completely. Cell Adapters in the Instrument period will begin.
Page 87
Aluminum (continued) Interfering Substance Interference Levels , Cr 0.5 mg/L – 0.1 mg/L Higher concentrations of heavy metals than those given, as well as fluoride, phosphate and relatively rare elements such as beryllium, thorium, titanium, zirconium and vanadium interfere with the determination. Aluminum oxide hydrates and hydroxide are only partially determined.
Page 89
These materials should not be poured down the drain. See Section 4 of this manual for more information on proper disposal of these materials. Method 8013 Hach Programs User Program Perform the User Touch Prepare the Hach Dampen a cotton ball Programming procedure Distillation Apparatus with 10% Lead Acetate User Program on page 5.
Page 90
Arsenic Heat control: 0 Text Below Prepare the arsenic Using a graduated Using a graduated Turn on the power absorber solution as cylinder, pour 25-mL of cylinder, pour 250 mL of switch. Set the stir control directed under Reagent prepared arsenic sample into the to 5.
Page 91
Arsenic 25 mL 20 mL 10 mL Touch the timer icon. When the timer Rinse the gas bubbler Fill a dry, 25-mL beeps, turn off the heater. by moving it up and sample cell with Touch Remove the cylinder/gas down in the arsenic untreated arsenic A third 15-minute reaction bubbler assembly as a...
Page 92
Arsenic Reagent Preparation Prepare the arsenic absorber solution as follows: 1. Weigh 1.00 g of silver diethyldithiocarbamate on an analytical balance. 2. Transfer the powder to a 200-mL volumetric flask. Dilute to volume with pyridine. You must use pyridine only in a fume hood and wear chemical resistant gloves.
Page 93
Arsenic Calibration Standard Preparation Perform a new calibration for each lot of arsenic absorber solution. 1. Prepare a 10.0-mg/L arsenic working standard by pipetting 10.0 mL of Arsenic Standard Solution, 1000 mg/L As (Cat. No. 14571-42) into a 1000-mL volumetric flask. 2.
Page 95
• Twenty Antibody Cuvettes are provided with each reagent set. One Antibody Cuvette will be used for each calibrator and each sample. Cuvettes are not reusable. • Hach Company recommends wearing protective nitrile gloves for this procedure. Atrazine Page 1 of 8...
Page 96
Atrazine Immunoassay Procedure for Water λ Touch Label an Antibody Place the cuvettes Pipet 0.5 mL of each Cuvette for each into the rack snugly. calibrator into the Single Wavelength calibrator and each appropriately labeled λ then touch the button. sample to be tested.
Page 97
Atrazine At the end of the Wash each cuvette 20-minute period, discard forcefully and thoroughly the contents of all the four times with deionized cuvettes into an water. Empty the rinse appropriate waste water into the waste container. container. Note: Ensure most of the water is drained from the cuvettes by turning the cuvettes upside down and tapping them lightly...
Page 98
Atrazine Measuring the Color Zero Label and fill a Install the 1-cm Touch Place the first Zero Zeroing Cuvette with square cell adapter. calibrator into the The display will show: deionized water. Wipe celladapter. Note: See Section 2.6 Sample 0.000 Abs the outside of all the Cell Adapters in the Instrument Touch...
Page 99
Atrazine Using the 1-cm MicroCuvette Rack This rack (see Figure 2) has been designed specifically to aid in achieving precise and accurate results when using the immunoassay technique to analyze several samples at the same time. Figure 2 The 1-cm MicroCuvette Rack Loading the Rack —...
Page 100
Atrazine Interpretation Sample #1 — Sample reading is less than the readings for both calibrators. Therefore the sample concentration of Atrazine is greater than both 0.5 ppb and 3.0 ppb Atrazine. Sample #2 — Sample reading is between the readings for the 0.5 ppb and 3.0 ppb Atrazine calibrators.
Page 101
® TenSette , Pipet, 0.1–1.0 mL....................each....19700-01 Tips, for pipettor 19700-01....................1000/pkg...21856-28 Optional Reagents Reagent Set, Atrazine ......................100 cuvettes ..27627-10 * Immunoassay components are manufactured for Hach Company by Beacon Analytical Systems, Inc. Atrazine Page 7 of 8 ATZ_None_Other_IMM_Eng_Ody.fm...
Page 103
• Immediately after each test, clean the sample cell with soap, water, and a brush to prevent a film of barium from forming inside the sample cell. Powder Pillows Method 8014 Hach Programs 25 mL 25 mL 20 mL 20 mL...
Page 104
Touch Read Results will appear in mg/L Ba AccuVac Ampul Method 8014 Hach Programs 25 mL 20 mL 10 mL Touch Fill a round sample Fill a barium Quickly invert the ® cell with 25-mL of sample...
Page 105
Barium 25 mL 20 mL Zero 10 mL Touch the timer icon. When the timer Touch Within five minutes Zero beeps, place the blank after the timer beep, Touch The display will show: into the cell holder. place the prepared A five-minute reaction 0 mg/L Ba sample into the cell...
Page 106
Barium Standard Solutions Prepare a 90.0-mg/L barium standard solution as follows: 1. Pipet 9.00 mL of Barium Standard Solution, 1000-mg/L, into a 100-mL volumetric flask. 2. Dilute to the mark with deionized water. 3. Prepare this solution daily. Perform the barium procedure as described above. To adjust the calibration curve using the reading obtained with the 90.0-mg/L standard solution: 1.
Page 107
Barium Method Performance Standard: 30 mg/L Ba Program 95% Confidence Limits of Distribution 25–35 mg/L Ba 25–35 mg/L Ba See Section 3.4.3 Precision on page 44 for more information, or if the standard concentration did not fall within the specified range. Sensitivity ∆Abs ∆Concentration...
Page 109
), add 10 drops of Rochelle Salt Solution (Cat. No. 1725-33) before adding reagent. • Avoid fingerprints on the quartz surface of the lamp. Rinse the lamp and wipe with a soft, clean tissue between tests. Powder Pillows Method 8079 Hach Programs 25 mL 25 mL 20 mL 20 mL...
Page 110
Benzotriazole or Tolyltriazole 25 mL 20 mL 10 mL Put on UV safety Insert the ultraviolet Touch the timer icon. When the timer goggles. lamp into the sample cell. beeps, turn the lamp off. Touch Remove the lamp from Turn on the UV lamp. A 5-minute reaction the cell (the prepared period will begin.
Page 111
Benzotriazole or Tolyltriazole Interferences (continued) Interfering Substance Interference Levels and Treatments Chromium (as chromate) Greater than 12 mg/L Copper Greater than 10 mg/L Greater than 500 mg/L as CaCO . Add 10 drops of Rochelle Salt Solution (Cat. No. 1725-33) Hardness before adding reagent.
Page 113
• Sulfuric acid may contain residual moisture; this will cause low results. It is advisable to ensure sulfuric acid suitability by running a known boron standard before running any unknown samples. Powder Pillows Method 8015 Hach Programs Touch Using a 100-mL Add the contents of...
Page 114
Boron 25 mL 25 mL 20 mL 20 mL 10 mL 10 mL Accurately pipet Using a 50-mL Touch the timer icon. When the timer 2.0 mL of sample into graduated cylinder, add beeps, pour at least Touch another 125-mL 35 mL of the solution 10 mL from each flask A 25-minute reaction...
Page 115
Boron The BoroVer 3/Sulfuric Acid Solution is highly acidic. Neutralize to pH 6–9 and flush down the drain for disposal. For more information on waste management, see Section 4. Accuracy Check Standard Additions Method (Sample Spike) 1. After reading test results, leave the unspiked sample in the instrument. Verify the chemical form.
Page 117
• Sample temperature should be 22–24 °C (72–75 °F) for most accurate results. If outside this range, measure and record the sample temperature. See Sample Temperature Compensation on page 4. Powder Pillows Method 10061 Hach Programs Touch Fill a clean plastic Fill a second clean...
Page 118
Boron Open one pillow Cap the prepared Touch the timer icon. Continue shaking ™ BoroTrace 2 Reagent sample and shake to vigorously for Touch and add the contents to dissolve the powder. 30 seconds, or until all A ten-minute reaction the prepared sample.
Page 119
Boron Zero Read Place the blank into Touch Place the prepared Touch Zero Read the cell holder. sample into the cell The display will show: Results will appear in holder. mg/L B. 0.00 mg/L B Cell Matching Procedure 1. Rinse and fill two cells with deionized water. 2.
Page 120
Sample Temperature Compensation The reaction chemistry is very dependent on the sample temperature. Hach calibrations are performed at 23 °C (73 °F). If the sample temperature is outside the range of 22–24 °C (72–75 °F), multiply the results, in mg/L, by the appropriate multiplier (Table 3).
Page 121
Boron Table 3 Sample Temperature Multipliers Sample Temp. Sample Temp. Multiplier Multiplier °C °F °C °F 0.70 0.94 0.73 1.04 0.78 1.06 0.81 1.08 0.84 1.10 0.87 1.12 0.91 1.15 Accuracy Check Standard Additions Method (Sample Spike) 1. After reading test results, leave the sample cell (unspiked sample) in the instrument.
Page 123
• Wipe the outside of sample cells before each insertion into the instrument cell holder. Use a damp towel followed by a dry one to remove fingerprints or other marks. Powder Pillows Method 8016 Hach Programs Touch Fill a sample cell with Add the contents of Touch the timer icon.
Page 124
Touch Read Results will appear in mg/L Br ® AccuVac Ampul Method 8016 Hach Programs Touch Fill a sample cell with Fill a DPD Total Quickly invert the 10 mL of sample. (This is Chlorine Reagent ampules several times to Hach Programs the blank.)
Page 125
Bromine Zero 10 mL Touch the timer icon. Wipe the blank and Touch Within three minutes Zero place it into the cell after the timer beeps, Touch The display will show: holder. wipe the ampul and place A three-minute reaction 0.00 mg/L Br it into the cell holder.
Page 127
• Make sure that the temperature of the sample and the reagents is between 15–25 °C. • Underrange appears on the display when the instrument is zeroed or when the determined sample concentration is below the operating range listed for this method. UniCell Vials Hach Programs Touch Pipet 10.0 mL of Pipet 1.0 mL of...
Page 128
Cadmium Zero Pipet 0.5 mL of Close the sample vial Install the 16-mm cell Touch Zero Stabilizer B (HCT 154 B) and invert several times adapter. The display will show: into a sample vial. to mix. Note: See Section 2.6 Sample 0.00 mg/L Free Cd Cell Adapters in the Instrument Underrange...
Page 129
Cadmium Total cadmium, including undissolved cadmium and complexed cadmium can only be determined after digesting with the Metal Prep Set, HCT 200. Note: The total cadmium measuring range is 0.02–0.36 mg/L. Sample Collection, Storage, and Preservation Collect samples in acid-cleaned glass or plastic containers. No acid addition is necessary if analyzing the samples immediately.
Page 131
• Wipe the outside of sample cells before each insertion into the instrument cell holder. Use a damp towel followed by a dry one to remove fingerprints or other marks. Test “N Tube Method 10172 Zero Hach Programs Touch Remove the cap from Install the 16-mm cell Touch...
Page 132
Chloramine (Mono) Read Remove the vial from Touch the timer icon. After the color has Touch Read the adapter. Using a developed fully, place the Touch Results will appear in micro-funnel, add the vial into the cell adapter. mg/L Cl A 5-minute reaction contents of one period will begin.
Page 133
Chloramine (Mono) Table 1 Non-interfering Substances (continued) Substance Maximum Level Tested Nitrate 100 mg/L N Nitrite 50 mg/L N Phosphate 100 mg/L PO Silica 100 mg/L SiO Sulfate 2600 mg/L 2– Sulfite 50 mg/L SO Tyrosine 1 mg/L N Urea 10 mg/L N Zinc 5 mg/L...
Page 134
Chloramine (Mono) 7. Open an ampule and use a glass Mohr pipet to add the calculated amount of Chlorine Solution slowly to the ammonia standard, while mixing at medium speed on a stir-plate. 8. Allow the monochloramine solution to mix for 1 minute after all Chlorine Solution is added.
Page 135
Chloramine (Mono) Safety Good safety habits and laboratory techniques should be used throughout the procedure. Consult the Material Safety Data Sheet (MSDS) for information specific to the reagent used. Required Reagents Quantity Required Description Per Test Unit Cat. No. HR Monochloramine Test ‘N Tubes, 50 tests ....................28051-45 Includes: ............................* (50) HR Monochloramine Diluent Vials...
Page 137
• Install the Multi-pathlength Cell into the adapter oriented for the short (1-cm) pathlength (the long pathlength is perpendicular to the front of the instrument). DR/2400 Multi-Path Cell Method 10171 Zero Hach Programs Touch Fill the Install the adapter. Touch...
Page 138
Chloramine (Mono) Read Remove the cell from Touch the timer icon. After the color has Touch Read theadapter and add the developed fully, wipe the Touch Results will appear in contents of one pillow cell and place it into the mg/L Cl A 5-minute reaction Monochlor-F to the...
Page 139
Chloramine (Mono) Table 1 (continued) Substance Maximum Level Tested Phosphate 100 mg/L PO Silica 100 mg/L SiO Sulfate 2600 mg/L 2– Sulfite 50 mg/L SO Tyrosine 1 mg/L N Urea 10 mg/L N Zinc 5 mg/L Table 2 Interfering Substance Recommended Interference Level and its effect...
Page 140
Chloramine (Mono) Accuracy Check To check test accuracy, prepare the following 4.5-mg/L (as Cl ) monochloramine standard fresh before use. 1. Add the contents of one Buffer Powder Pillow, pH 8.3, to about 50-mL of organic-free water in a clean 100-mL Class A volumetric flask. Swirl to dissolve the powder.
Page 141
Chloramine (Mono) Sensitivity ∆Abs ∆Concentration Portion of Curve Entire range 0.010 0.04 mg/L Cl See Section 3.4.5 Sensitivity on page 43 for more information. Summary of Method In the presence of a cyanoferrate catalyst, monochloramine (NH Cl) in the sample reacts with a substituted phenol to form an intermediate monoimine compound.
Page 143
• Wipe the outside of sample cells before each insertion into the instrument cell holder. Use a damp towel followed by a dry one to remove fingerprints or other marks. Method 8113 Hach Programs 25 mL 25 mL 25 mL...
Page 144
Chloride 25 mL 25 mL 25 mL 25 mL 20 mL 20 mL 20 mL 20 mL 25 mL 25 mL 20 mL 20 mL 10 mL 10 mL 10 mL 10 mL 10 mL 10 mL Swirl to mix. Pipet 1.0 mL of Ferric Swirl to mix.
Page 145
Chloride Sample Collection, Storage, and Preservation Collect samples in glass or plastic containers. Samples can be stored for at least 28 days at room temperature. Accuracy Check Standard Additions Method (Sample Spike) 1. After reading test results, leave the sample cell (unspiked sample) in the instrument.
Page 147
• Analyze samples immediately because chlorine dioxide is unstable and volatile. See Interferences. • Wipe the outside of sample cells before each insertion into the instrument cell holder. Use a damp towel followed by a dry one to remove fingerprints or other marks. Method 8138 Hach Programs Zero 10 mL Touch...
Page 148
Chlorine Dioxide Interferences Interfering Substance Interference Levels and Treatments 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 (Cat. No. 1045-32). Determine amount to be added on Acidity separate sample aliquot, then add the same amount to the sample being tested.
Page 149
Only a trained chemist should prepare the standards using appropriate safety equipment and precautions. Hach does not recommend preparation of chlorine dioxide standards. If independent standard preparation is required, please see the instructions in Standard Methods for the Examination of Water and Wastewater, 20th ed., under the...
Page 151
Dilute the sample with high quality water that is chlorine demand-free, and repeat the test. Some loss of chlorine dioxide may occur. Multiply the result by the appropriate dilution factor. Powder Pillows Method 10126 Hach Programs Zero 10 mL Touch...
Page 152
Read 20 seconds to mix. Results will appear in mg/L ClO ® AccuVac Ampul Method 10126 Zero Hach Programs 10 mL 10 mL Touch Fill a round sample Wipe the blank and Touch Zero cell with 10-mL of place it into the cell...
Page 153
Chlorine Dioxide Add 16 drops of Fill a DPD Free Quickly invert the Within one minute of Glycine Reagent to the Chlorine Reagent ampule several times to adding the sample, wipe sample in the beaker. AccuVac Ampul with mix. Wait 30 seconds for the ampule and place it Swirl gently to mix.
Page 154
Chlorine Dioxide Interfering Substance Interference Levels and Treatments Various metals may interfere by combining with the glycine needed to remove the chlorine interference. Metal interference is limited except when chlorine is present. In the presence of Metals 0.6 mg/L Cl , both copper (>10 mg/L) and nickel (>50 mg/L) interfere.
Page 155
Dilute 1 drop of 5% chlorine bleach in 1 liter of chlorine-demand-free deionized water. Use this as the standard. b. Verify the standard’s concentration using the Hach Free Chlorine Method 8021. c. Perform the chlorine dioxide test on the standard without adding glycine.
Page 157
® • A TenSette pipet (Cat. No. 19700-01) may be used to dispense Chlorine Dioxide Reagent A. Amaranth Method Hach Programs 10 mL Touch Using the syringe and Fill the volumetric Pour 10 mL from the...
Page 158
Chlorine Dioxide 10 mL Add 1.0 mL of Fill the second Touch the timer icon. Pour 10 mL from the Chlorine Dioxide volumetric flask to the Touch . A 1-minute second volumetric flask Reagent A into a second mark with the sample. reaction period will into a second sample cell.
Page 159
Only a trained chemist should prepare the standards using appropriate safety equipment and precautions. Hach does not recommend preparation of chlorine dioxide standards. If independent standard preparation is required, please see the instructions in Standard Methods for the Examination of Water and Wastewater, 20th ed., under...
Page 161
® • A TenSette pipet (Cat. No. 19700-01) may be used to dispense Chlorine Dioxide Reagent 1 and Chlorine Dioxide Reagent 3. Powder Pillows Method 8065 Hach Programs Touch Fill two 50-mL Use a volumetric Add the contents of mixing cylinders to the...
Page 162
Chlorine Dioxide Use a Class A pipet to Invert several times Use a volumetric Invert several times add exactly 1.00 mL of to mix. pipet and pipet filler to to mix. Chlorine Dioxide add 1.0 mL of Chlorine Reagent 2 to each Dioxide Reagent 3 to each cylinder.
Page 163
Only a trained chemist should prepare the standards using appropriate safety equipment and precautions. Hach does not recommend preparation of chlorine dioxide standards. If independent standard preparation is required, please see the instructions in Standard Methods for the Examination of Water and Wastewater, 20th ed., under the...
Page 165
• Wipe the outside of sample cells before each insertion into the instrument cell holder. Use a damp towel followed by a dry one to remove fingerprints or other marks. Powder Pillows Method 8021 Hach Programs Zero 10 mL Touch...
Page 166
Swirl the sample cell for 20 seconds to mix. Proceed to step 7 immediately. ® AccuVac Ampul Method 8021 Hach Programs Zero 10 mL 10 mL Touch Fill a round sample Wipe the blank and Touch Zero cell with 10-mL of...
Page 167
Chlorine, Free Read Fill a DPD Free Quickly invert the Within one minute of Touch Read Chlorine Reagent ampule several times to sample addition, wipe Results will appear in AccuVac Ampul with mix. Wipe off any liquid the AccuVac Ampul and mg/L Cl sample.
Page 168
Chlorine, Free Sample Collection, Storage and Preservation Analyze samples for chlorine immediately after collection. Free chlorine is a strong oxidizing agent and it 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 169
Chlorine, Free 7. After completing the sequence, touch to view the best-fit line through Graph the standard additions data points, accounting for matrix interferences. Touch , then select and touch to view the relationship between View: Fit Ideal Line the sample spikes and the “Ideal Line” of 100% recovery. See Section 3.2.2 Standard Additions on page 32 for more information.
Page 171
• Install the Multi-pathlength Cell into the adapter oriented for the short (1-cm) pathlength (the long pathlength is perpendicular to the front of the instrument). DR/2400 Multi-Path Cell Method 10069 Zero Hach Programs Touch Fill the Install the adapter. Touch...
Page 172
Chlorine, Free Read Remove the cell from Place the prepared Touch Read the adapter and add the sample into the adapter. Results will appear in contents of one DPD Free mg/L Cl Chlorine powder pillow to the sample. Cap and shake the cell about 20 seconds to dissolve.
Page 173
Chlorine, Free Interfering Substance Interference Levels and Treatments Ozone Interferes at all levels Peroxides May interfere Extreme sample pH or highly Adjust to pH 6 –7 using acid (Sulfuric Acid, Cat. No. 1270-32) or base (Sodium Hydroxide, buffered samples Cat. No. 1045-32). * Samples treated with sodium arsenite for interferences will be hazardous waste as regulated by the Federal RCRA for arsenic (D004).
Page 175
• Install the Pour-Thru Cell into the adapter so that the long pathlength (1-in./25-mm) is parallel to the front of the instrument. DR/2400 Pour-Thru Cell Method 10059 Zero Hach Programs Touch Install the Pour-Thru Pour approximately When the flow stops,...
Page 176
Chlorine, Free Add 1.0 mL of Free Add 1.0 mL of Carefully fill the Fill the funnel of the Chlorine Buffer Solution prepared Free Chlorine mixing cylinder to the Pour-Thru Cell with the to a clean, dry 100-mL Indicator Solution to the 80-mL mark with sample.
Page 177
Chlorine, Free Reagent Preparation The Free Chlorine Indicator Solution must be prepared before use. Using a powder funnel, add the contents of one 24 g bottle of DPD Powder (Cat. No. 22972-55) to one 473-mL bottle of Free Chlorine Indicator Solution (Cat.
Page 178
Chlorine, Free If sample containers are rinsed thoroughly with deionized water after use, only occasional pretreatment is necessary. A pre-treated BOD bottle with a ground- glass stopper makes an ideal sample container for chlorine analysis. Treating Analysis Labware Glassware used in this test must be chlorine demand-free. Fill the 100-mL mixing cylinder and sample container with a dilute solution of chlorine bleach prepared by adding 1 mL of commercial bleach to 1 liter of water.
Page 179
Chlorine, Free Method Performance Precision Standard: 1.07 mg/L Cl Program 95% Confidence Limits of Distribution 1.05–1.09 mg/L Cl See Section 3.4.3 Precision on page 44 for more information, or if the standard concentration did not fall within the specified range. Sensitivity ∆Abs ∆Concentration...
Page 181
Touch Zero Test ‘N Tube™ vial to the adapter. The display will show: Hach Programs top of the Hach label with Note: See Section 2.6 Sample Select program 0.00 mg/L Cl sample (This is the Cell Adapters in the Instrument blank.)
Page 182
(This is the mg/L Cl sample to the tube. (Fill prepared sample). the vial to the top of the Hach label. Interferences Interfering Substance Interference Levels and Treatments Greater than 150 mg/L CaCO . May not develop full color or color may fade instantly. Neutralize to pH 6–7 with1 N sodium hydroxide.
Page 183
Chlorine, Free (continued) Interfering Substance Interference Levels and Treatments 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.Typical interference levels of monochloramine in the free chlorine test are listed below (as mg/L Cl Sample Temp.
Page 185
• Wipe the outside of sample cells before each insertion into the instrument cell holder. Use a damp towel followed by a dry one to remove fingerprints or other marks. Powder Pillows Method 8167 Hach Programs Touch Fill a round sample Add the contents of Touch the timer icon.
Page 186
Wipe the sample cell and place it into the cell holder. ® AccuVac Ampul Method 8167 Hach Programs 10 mL Touch Fill a round sample Fill a DPD Total Quickly invert the cell with 10-mL of sample...
Page 187
Chlorine, Total Zero 10 mL Touch the timer icon. Wipe the blank and Touch . The Within three minutes Zero place it into the cell display will show: after the timer beep, wipe Touch holder. the AccuVac Ampul and 0.00 mg/L Cl A three-minute reaction place it into the cell period will begin.
Page 188
Chlorine, Total Sample Collection, Storage and Preservation Analyze samples for chlorine immediately after collection. Free chlorine is a strong oxidizing agent and it 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 189
Chlorine, Total 7. After completing the sequence, touch to view the best-fit line through Graph the standard additions data points, accounting for matrix interferences. Touch , then select and touch to view the relationship between View: Fit Ideal Line the sample spikes and the “Ideal Line” of 100% recovery. See Section 3.2.2 Standard Additions on page 32 for more information.
Page 191
• Install the Multi-pathlength Cell into the adapter oriented for the short (1-cm) pathlength (the long pathlength is perpendicular to the front of the instrument). DR/2400 Multi-Path Cell Method 10070 Zero Hach Programs Touch Fill the Install the adapter. Touch...
Page 192
Chlorine, Total Read Remove the cell from Touch the timer icon. After the color has Touch Read the adapter and add the developed fully, wipe the Touch Results will appear in contents of one DPD cell and place it into the mg/L Cl A 3-minute reaction Total Chlorine powder...
Page 193
Chlorine, Total 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 free chlorine in water. Avoid plastic containers since these may have a large chlorine demand.
Page 195
• Install the Pour-Thru Cell into the adapter so that the long pathlength (1-in./25-mm) is parallel to the front of the instrument. DR/2400 Pour-Thru Cell Method 10060 Zero Hach Programs Touch Install the Pour-Thru Pour approximately When the flow stops,...
Page 196
Chlorine, Total Add 1.0 mL of Total Add 1.0 mL of Carefully fill the Touch the timer icon. Chlorine Buffer Solution prepared Total Chlorine mixing cylinder to the Touch to a clean, dry 100-mL Indicator Solution to the 80-mL mark with sample. A two-minute reaction glass mixing cylinder same mixing cylinder...
Page 197
Chlorine, Total Reagent Preparation The Total Chlorine Indicator Solution must be prepared before use. Using a powder funnel, add the contents of one 24 g bottle of DPD Powder (Cat. No. 22972-55) to one 473-mL bottle of Total Chlorine Indicator Solution (Cat.
Page 198
Chlorine, Total Treating Analysis Labware Glassware used in this test must be chlorine demand-free. Fill the 100 mL mixing cylinder and sample container with a dilute solution of chlorine bleach prepared by adding 1 mL of commercial bleach to 1 liter of water. Soak in this solution at least one hour.
Page 199
Chlorine, Total Method Performance Precision Standard: 1.07 mg/L Cl Program 95% Confidence Limits of Distribution 1.06–1.08 mg/ L Cl See Section 3.4.3 Precision on page 44 for more information, or if the standard concentration did not fall within the specified range. Sensitivity ∆Abs ∆Concentration...
Page 201
See Determining the Reagent Blank Value on page 3. To store the reagent blank value, see Creating a User Program Based on a Hach Program in the instrument manual.
Page 202
Chlorine, Total Zero ® When the timer Break open one ULR Using a TenSette Break open one beeps, touch Chlorine Buffer Solution Pipet and a clean tip, ampule of DPD Indicator Zero Ampule. transfer 1.0 mL of buffer Solution for Ultra Low The display will show: from the ampule to a Range Chlorine.
Page 203
Flush the Pour-Thru Cell with at least 50 mL of deionized water immediately after use. Determining the Reagent Blank Value Options Hach Programs Reagent Blank: Touch Make sure that the Install the Pour-Thru Collect about 100 mL reagent blank setting is...
Page 204
Chlorine, Total General Timer ® Using a TenSette Touch the timer icon, After the timer beeps, Break open one Pipet, add 1.0 mL of then the break open one ampule ampule of DPD Indicator General Timer Blanking Reagent to the option.
Page 205
When the timer beeps, Use this value to Note: See Creating a User Flush the Pour-Thru Program Based on a Hach introduce the contents of correct the sample result Cell with at least 50 mL of Program in the instrument...
Page 206
Chlorine, Total Sample Collection, Storage, and Preservation Analyze samples for chlorine immediately after collection. Many factors, including reactant concentrations, sunlight, pH, temperature and salinity influence decomposition of chlorine in water. Avoid plastic containers since these may have a large chlorine demand. Pretreat glass sample containers to remove any chlorine demand by soaking in a dilute bleach solution (0.5 mL commercial bleach to l liter of deionized water) for at least 1 hour.
Page 207
Chlorine, Total 5. Prepare three sample spikes. Fill three mixing cylinders (Cat. No. 1896-41) ® with 50 mL of sample. Use the TenSette Pipet to add 0.1 mL, 0.2 mL, and 0.3 mL of standard, respectively, to each sample and mix thoroughly. 6.
Page 209
Determining the Reagent Blank Value on page 4. To store the reagent blank value, see Creating a User Program Based on a Hach Program in the instrument manual. • The reagent blank value is normally less than 5 µg/L. If the value is greater than 5 µg/L, an interfering substance may be present in the blanking water or the DPD Indicator may be degrading.
Page 210
Chlorine, Total ® ® Break open one ULR Using a TenSette Break open one Using a TenSette Chlorine Buffer Solution Pipet and a clean tip, ampule of DPD Indicator Pipet and a clean tip, Ampule. transfer 1.0 mL of buffer Solution for Ultra Low transfer 1.0 mL of from the ampule to a...
Page 211
Chlorine, Total Zero Pour the filtered After the flow stops, Pull the barrel’s valve Push the barrel’s sample from the plunger touch button out to the “open” valve button to the Zero reservoir into the position. Pull the plunger “closed” position. Place The display will show: Pour-Thru Cell.
Page 212
Below Determine a reagent blank using the procedure following these steps. Determining the Reagent Blank Value Options Hach Programs Reagent Blank Touch Make sure that the Install the Pour-Thru Collect about 100 mL reagent blank setting is Cell and multi-...
Page 213
Chlorine, Total General Timer ® Using a TenSette Touch the timer icon, After the timer beeps, Break open one Pipet, add 1.0 mL of then the break open one ampule ampule of DPD Indicator General Timer Blanking Reagent to the option.
Page 214
Chlorine, Total When the timer Use this value to Flush the Pour-Thru beeps, introduce the correct the sample result Cell with at least 50 mL of contents of the cylinder obtained in this deionized water into the Pour-Thru Cell. procedure. immediately after use.
Page 215
Chlorine, Total Sample Collection, Storage and Preservation Analyze samples for chlorine immediately after collection. Free chlorine is a strong oxidizing agent and it 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 chlorine in water.
Page 216
Chlorine, Total 5. Prepare three sample spikes. Fill three mixing cylinders (Cat. No. 1896-41) ® with 50 mL of sample. Use the TenSette Pipet to add 0.1 mL, 0.2 mL, and 0.3 mL of standard, respectively, to each sample and mix thoroughly. 6.
Page 217
Chlorine, Total Required Reagents Quantity Required Description Per Test Unit Cat. No ULR Chlorine Reagent Set (about 20 tests) ....................25630-00 Includes: ULR Chlorine Buffer Solution, 1.5 mL ampules......1 mL ....20/pkg....24931-20 DPD Indicator Solution for ULR Chlorine, 1.5 mL ampules ..1 mL ....20/pkg....24932-20 Blanking Reagent for ULR Chlorine ..........
Page 219
Install the 16-mm Test ‘N Tube™ vial to the the vial with a damp adapter. Hach Programs top of the Hach label with towel, then a dry towel to Note: See Section 2.6 Sample Select program sample. (This is the...
Page 220
10 mL of sample to the inversions should take at period will begin. tube. (Fill the vial to the least 30 seconds. One top of the Hach label.) inversion equals turning the vial upside down, This is the prepared then returning it to an sample.
Page 221
Chlorine, Total (continued) Interfering Substance Interference Levels and Treatments Hardness No effect at less than 1,000 mg/L as CaCO Iodine, I Interferes at all levels 1. Adjust sample pH to 6–7. 2. Add 3 drops Potassium Iodide (30-g/L) (Cat. No. 343-32) to a 25-mL sample. Manganese, oxidized 3.
Page 223
• The final samples are highly acidic. Neutralize to pH 6–9 with Sodium Hydroxide Standard Solution (Cat. No. 2450-26) and flush down the drain for disposal. For more information on pollution prevention and waste management, refer to Section 4. Powder Pillows Method 8023 Hach Programs Touch Fill a round sample Add the contents of Touch the timer icon.
Page 224
0.00 mg/L Cr Touch Read Results will appear in mg/L Cr AccuVac Ampul Method 8023 Hach Programs 10 mL Touch Fill a round sample Fill a ChromaVer 3 Quickly invert the cell with 10-mL of sample Reagent AccuVac® ampule several times to Hach Programs (the blank).
Page 225
Chromium, Hexavalent Zero 10 mL Touch the timer icon. When the timer Touch Place the prepared Zero beeps, place the blank sample into the cell Touch The display will show: into the cell holder. holder. A five-minute reaction 0.00 mg/L Cr6+ Touch Read period will begin.
Page 226
Chromium, Hexavalent ® 5. For analysis using powder pillows, use the TenSette Pipet to add 0.1 mL, 0.2 mL, and 0.3 mL of standard, respectively to three 25-mL samples and mix thoroughly. Transfer 10 mL of each solution into a 10-mL sample cell and analyze as described above.
Page 227
Chromium, Hexavalent Summary of Method Hexavalent chromium is determined by the 1,5-Diphenylcarbohydrazide method using a single dry powder formulation called ChromaVer 3 Chromium Reagent. This reagent contains an acidic buffer combined with 1,5-Diphenylcarbohydrazide, which reacts to give a purple color when hexavalent chromium is present.
Page 229
• Make sure that the temperature of the water sample and the sample vial is between 15–25 °C • Underrange appears on the display when the instrument is zeroed or when the determined sample concentration is below the operating range listed for this method. UniCell Vials Hach Programs Touch Pipet 4.0 mL of Cap the sample vial...
Page 230
Chromium, Hexavalent Zero Touch the timer icon. Install the 16-mm cell Touch Wipe the sample vial Zero adapter. and place it into the cell Touch The display will show: adapter. Note: See Section 2.6 Sample A five-minute reaction 0.00 mg/L Cr Cell Adapters in the Instrument Touch Read...
Page 231
Chromium, Hexavalent Sample Collection, Preservation, and Storage Collect samples in a cleaned glass or plastic container. Store at 4 °C (39 °F) up to 24 hours. Samples must be analyzed within 24 hours. Accuracy Check Standard Additions Method (Sample Spike) 1.
Page 233
• Prepare a boiling water bath for step 4. • Use finger cots (Cat. No. 14647-02) to handle hot sample cells. • Undissolved powder does not affect accuracy. Powder Pillows Method 8024 Hach Programs 25 mL 25 mL 20 mL 20 mL...
Page 234
Chromium, Total 25 mL 25 mL 20 mL 20 mL 10 mL 10 mL Touch the timer icon. When the timer Remove cap and add Remove cap and add beeps, remove the the contents of one the contents of one Acid Touch prepared sample.
Page 235
Chromium, Total Interferences Interfering Substance Interference Levels and Treatments Highly buffered samples or May exceed the buffering capacity of the reagents and require sample pretreatment; see Section extreme sample pH 3.3 Interferences on page 41. May inhibit complete oxidation of trivalent chromium. If high levels of organic material are Organic material present, see Section 4 for instructions on sample digestion.
Page 237
• Make sure that the temperature of the water sample and the sample vial is between 15–25 °C. • Underrange appears on the display when the instrument is zeroed or when the determined sample concentration is below the operating range listed for this method. UniCell Vials Hach Programs Touch Pipet 4.0 mL of Screw a blue...
Page 238
Chromium, Total HRS MIN SEC HRS MIN SEC Heat the vial in After the heating When the vials have Touch the timer icon. the reactor block for period, remove the vial cooled to room Touch 60 minutes at 100 °C. from the reactor block temperature, screw an A 10-minute reaction...
Page 239
Chromium, Total (continued) Interfering Substance Interference Levels , Pb 25 mg/L , Fe 10 mg/L 1 mg/L Larger amounts of iron, copper, reducing or oxidizing agents give low results. Lead, mercury, and tin give high results. Note: Undissolved chromium is not determined with the determination of chromium VI. Total Chromium can only be determined after digestion.
Page 241
• Wipe the outside of sample cells before each insertion into the instrument cell holder. Use a damp towel followed by a dry one to remove fingerprints or other marks. Powder Pillows Method 8078 Hach Programs 10 mL Touch Fill a round sample...
Page 242
Cobalt 10 mL Use the plastic Touch the timer icon. When the timer Place the blank into dropper provided to add beeps, add the contents of the cell holder. Touch 0.5 mL of 0.3% PAN one EDTA Reagent A three-minute reaction Indicator Solution to each Powder Pillow to each period will begin.
Page 243
Cobalt Interferences Interfering Substance Interference Levels and Treatments 32 mg/L 1000 mg/L as CaCO 20 mg/L – 8000 mg/L 20 mg/L 40 mg/L 15 mg/L – 20 mg/L Interferes directly and must not be present 10 mg/L 500 mg/L 400 mg/L 25 mg/L 60 mg/L 5000 mg/L...
Page 245
120 Color, 455 nm Note: NCASI prescribes a 0.8-micron filter. 125 Color, 465 nm Touch Start Note: Use Hach program 125 when performing the NCASI procedure. Color, True and Apparent Page 1 of 4 ColorTru_None_Other_PCS_Eng_Ody.fm...
Page 246
Color, True and Apparent 10 mL 10 mL Pour another 50 mL Fill a round sample Pour about 50 mL of Fill a second round of deionized water cell with 10 mL of filtered sample through the filter. sample cell with 10 mL of through the filter.
Page 247
Color, True and Apparent Accuracy Check Standard Solution Method Prepare a 250 platinum-cobalt units standard as follows: 1. Using Class A glassware, pipet 50.00 mL of a 500 Platinum-Cobalt Units Standard Solution into a 100-mL volumetric flask. Dilute to the 100 mL mark with deionized water.
Page 249
• If copper is present, the sample will turn purple when it mixes with the reagent powder. • Accuracy is not affected by undissolved powder. Powder Pillows Method 8506 Hach Programs Touch Fill a sample cell with Add the contents of Touch the timer icon.
Page 250
0.00 mg/L Cu sample. Place the blank sample into the cell into the cell holder. holder. AccuVac Ampul Method 8026 Hach Programs 25 mL 20 mL 10 mL Touch Collect at least 40 mL Fill a CuVer 2 Quickly invert the...
Page 251
Copper 25 mL 20 mL Zero 10 mL Touch the timer icon. When the timer Touch Within 30 minutes Zero beeps, place the blank after the timer beeps, Touch The display will show: into the cell holder. Close place the AccuVac Ampul A 2-minute reaction 0.00 mg/L Cu the cover.
Page 252
Copper ® Table 2 Interfering Substances and Suggested Treatments for AccuVac Ampuls Interfering Substance Interference Levels and Treatments If the sample is extremely acidic (pH 2 or less) a precipitate may form. Add 8 N Potassium Acidity Hydroxide Standard Solution (Cat. No. 282-32) drop-wise until sample pH is above 4. Continue with step 2.
Page 253
Copper above. Accept each standard additions reading by touching Read. Each addition should reflect approximately 100% recovery. 8. After completing the sequence, touch to view the best-fit line through Graph the standard additions data points, accounting for matrix interferences. Touch , then select and touch to view the relationship between...
Page 255
• If samples contain high levels of metals, a slight metallic deposit or yellow buildup may form in the sample cell. Wash the cell as described above. Powder Pillows Method 8143 Hach Programs 10 mL Touch Fill two round sample...
Page 256
Copper Zero 10 mL 10 mL Add the contents of Touch the timer icon. When the timer Touch Zero one Porphyrin 2 Reagent beeps, place the blank Touch The display will show: Powder Pillow to each into the cell holder. A 3-minute reaction 0 µg/L Cu sample cell.
Page 257
Copper Interferences Interfering Substance Interference Levels and Treatments Aluminum, Al 60 mg/L Cadmium, Cd 10 mg/L Calcium, Ca 1500 mg/L Interfere at all levels unless either the Digesdahl or vigorous digestion is performed Chelating agents (see Section 4 on page 55). Chloride, Cl –...
Page 258
Copper 4. Touch to accept the default values for standard concentration, sample volume, and spike volumes. Touch to change these values. After values Edit are accepted, the unspiked sample reading will appear in the top row. See Standard Additions in the instrument manual for more information. ®...
Page 259
Copper Summary of Method The porphyrin method is very sensitive to trace amounts of free copper. The method is free from most interferences and does not require any sample extraction or concentration before analysis. Interferences from other metals are eliminated by the copper masking reagent. The porphyrin indicator forms an intense, yellow-colored complex with any free copper present in sample.
Page 261
• Underrange appears on the display when the instrument is zeroed or when the determined sample concentration is below the operating range listed for this method. UniCell Vials Hach Programs Touch Pipet 4 mL of sample Cap and invert the Touch the timer icon.
Page 262
Copper Zero Zero Install the 16-mm cell Touch Wipe the sample vial Touch Zero Read adapter. and place it into the cell The display will show: Results will appear in holder. Note: See Section 2.6 Sample mg/L Cu. 0.00 mg/L Free Cu Cell Adapters in the Instrument Underrange Manual for adapter installation...
Page 263
Copper Accuracy Check Standard Additions Method (Sample Spike) 1. After reading test results, leave the sample cell (unspiked sample) in the instrument. 2. Touch . Touch . A summary of the standard Options Standard Additions additions procedure will appear. 3. Touch to accept the default values for standard concentration, sample volume, and spike volumes.
Page 265
See Acid Distillation on page 5. • See Pollution Prevention and Waste Management on page 3 for proper disposal of solutions containing cyanide. Powder Pillows Method 8027 Hach Programs Touch Using a graduated Add the contents of...
Page 266
Cyanide Leave the sample cell Add the contents of Shake the sample for Add the contents of undisturbed for an one CyaniVer 4 Cyanide 10 seconds. Immediately one CyaniVer 5 Cyanide additional 30 seconds. Reagent Powder Pillow. proceed to step 8. Reagent Powder Pillow.
Page 267
Cyanide Pollution Prevention and Waste Management Special Considerations for Cyanide Containing Materials Samples analyzed by this procedure may contain cyanide, which is regulated as reactive (D003) waste by the federal RCRA. It is imperative these materials be handled safely to prevent the release of hydrogen cyanide gas (an extremely toxic material with the smell of almonds).
Page 268
Cyanide (continued) Interfering Interference Levels and Treatments Substance 1. Adjust a 25-mL portion of the alkaline sample to pH 7–9 with 2.5 N Hydrochloric Acid Standard Solution. (Cat. No. 1418-32) Count the number of drops added. 2. Add four drops of Potassium Iodide Solution (Cat. No. 343-32) and four drops of Starch Indicator Solution to the sample.
Page 269
Cyanide d. If step 3 suggests the presence of oxidizing agents, add two level, 1-g measuring spoonfuls of Ascorbic Acid (Cat. No. 6138-26) per liter of sample. e. Withdraw a 25-mL portion of sample treated with ascorbic acid and repeat steps 1 to 3. If the sample turns blue, repeat steps 4 and 5. f.
Page 270
(Cat. No. 22658-00) offered by Hach: a. Set up the distillation apparatus for cyanide recovery, leaving off the thistle tube. Refer to the Hach Distillation Apparatus Manual. Turn on the water and make certain it is flowing steadily through the condenser.
Page 271
Cyanide g. Using a water bottle, rinse the thistle tube with a small amount of deionized water. h. Allow the solution to mix for three minutes; then add 20 mL Magnesium Chloride Reagent (Cat. No. 14762-53) through the thistle tube and rinse again.
Page 273
• Make sure that the temperature of the water sample and the sample vial is between 15–25 °C (59–77 °F) • Underrange appears on the display when the instrument is zeroed or when the determined sample concentration is below the operating range listed for this method. UniCell™ Vials Hach Programs Touch Pipet 2 mL of sample Cap with grey Invert the sample vial into a sample vial.
Page 274
Cyanide Zero Pipet 2 mL of Touch the timer icon. Install the 16-mm cell Touch Zero Pyridine-hydrochloric adapter. Touch The display will show: acid B (HCT 129 B) into Note: See Section 2.6 Sample – An 8-minute reaction 0.00 mg/L CN the sample vial.
Page 275
Cyanide Accuracy Check Standard Additions Method (Sample Spike) Caution: cyanides and their solutions, and the hydrogen cyanide liberated by acids, are very poisonous. Both the solutions and the gas can be absorbed through the skin. – 1. Prepare a 100-mg/L CN stock solution weekly by dissolving 0.2503 grams, or an equivalent amount of pure potassium cyanide, in deionized water and diluting to 1000 mL.
Page 277
• After adding the reagent, a white turbidity will form if cyanuric acid is present. • Clean sample cells with soap, water, and a brush soon after each test to avoid a build-up of film on the sample cell. Powder Pillows Method 8139 Hach Programs 25 mL 25 mL 20 mL...
Page 278
Cyanuric Acid 25 mL 25 mL 20 mL 20 mL Zero Read 10 mL 10 mL Fill a second sample Touch Within seven minutes Touch Zero Read cell with 25 mL of sample after the timer beeps, The display will show: Results will appear in (the blank) and place it in place the prepared...
Page 279
Cyanuric Acid Method Performance Precision Standard: 10 mg/L cyanuric acid Program 95% Confidence Limits of Distribution 7–13 mg/L cyanuric acid See Section 3.4.3 Precision on page 44 for more information, or if the standard concentration did not fall within the specified range. Sensitivity ∆Abs ∆Concentration...
Page 281
• If the instrument displays OVER!, dilute a fresh sample (5 mL) with an equal volume of deionized water and repeat the test, using this solution in step 2. Multiply the result by 2. Using SPADNS Reagent Method 8029 Hach Programs 10 mL 10 mL 10 mL...
Page 282
Read period will begin. Results will appear in – mg/L F AccuVac Ampul Method 8029 Hach Programs Touch Collect at least 40 mL Fill one SPADNS Quickly invert the of sample in a 50-mL Fluoride Reagent ampules several times to Hach Programs beaker.
Page 283
Fluoride Zero Touch the timer icon. When the timer Touch Place the AccuVac Zero beeps, place the blank Ampul that contains the Touch The display will show: into the cell holder. sample into the cell – A one-minute reaction 0.00 mg/L F holder.
Page 284
Standard Solution Method A variety of standard solutions covering the entire range of the test is 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 285
Fluoride Method Performance Precision Standard: 1.00 mg/L F Program 95% Confidence Limits of Distribution – 0.95–1.05 mg/L F – 0.88–1.12 mg/L F See Section 3.4.3 Precision on page 44 for more information, or if the standard concentration did not fall within the specified range. Sensitivity ∆Concentration ∆Concentration...
Page 287
• Make sure that the temperature of the water sample and the sample vial is between 15–25 °C • Underrange appears on the display when the instrument is zeroed or when the determined sample concentration is below the operating range listed for this method. UniCell Vials Hach Programs Zero Touch Install the 16-mm cell...
Page 288
Fluoride Read Cap the sample vial Touch the timer icon. When the timer Touch Read and invert several times beeps, wipe the sample Touch Results will appear in to mix. vial and place it into the – mg/L F A 1-minute reaction celladapter.
Page 289
Fluoride 3. Touch to accept the default values for standard concentration, sample volume, and spike volumes. Touch to change these values. After values Edit are accepted, the unspiked sample reading will appear in the top row. See Standard Additions in the instrument manual for more information. 4.
Page 291
• Obtain formaldehyde-free water by distilling water from alkaline permanganate (4 g Sodium Hydroxide (Cat. No. 187-34), 2 g Potassium Permanganate (Cat. No. 769-05) per 500 mL of water). Discard the first 50–100 mL of distillate. Powder Pillows Method 8110 Hach Programs Touch Accurately measure Accurately measure...
Page 292
Formaldehyde Immediately touch Immediately after the Add the contents of Stopper the cylinder the timer icon. reaction period starts, one MBTH Powder and shake vigorously for shake the cylinder (the Pillow to the prepared 20 seconds. A 17-minute reaction blank) vigorously for sample when the timer period will begin.
Page 293
Formaldehyde Zero Read 10 mL 10 mL When the timer Pour the prepared Wipe the cell and When the timer shows , touch sample into a sample cell. place it into the cell beeps, touch 2:00 Zero Read Wipe the cell and place it holder.
Page 294
Formaldehyde Standard Additions Method (Sample Spike) 1. After reading test results, leave the sample cell (unspiked sample) in the instrument. 2. Touch . Touch . A summary of the standard Options Standard Additions additions procedure will appear. 3. Touch to accept the default values for standard concentration, sample volume, and spike volumes.
Page 295
Formaldehyde Formaldehyde reacts with MBTH (3-methyl-2-benzothiazoline hydrazone) and a developing solution to form a blue color in proportion to the formaldehyde concentration. Test results are measured at 630 nm. Required Reagents Quantity Required Description per test Unit Cat. No. Formaldehyde Reagent Set (100 Tests) ......................22577-00 Includes: (1) Developing Solution For Low Range Formaldehyde .....
Page 297
• Total hardness in mg/L equals mg/L Ca as CaCO plus mg/L Mg as CaCO • Remaining traces of EDTA or EGTA from previous tests will give erroneous results. Rinse sample cells thoroughly before using. Method 8030 Hach Programs Touch Pour 100 mL of Add 1.0 mL of...
Page 298
Note: This value is the amount of magnesium in the sample expressed as CaCO Exit 25 mL 20 mL Zero 10 mL Hach Programs Do not remove the Touch Touch Place the third cell Exit. Zero cell from the instrument.
Page 299
Hardness Interferences Interfering Substance Interference Levels and Treatments Chromium ( Above 0.25 mg/L Copper ( Above 0.75 mg/L EDTA, chelated Above 0.2 mg/L as CaCO Traces remaining in sample cells from previous tests will give erroneous results. Rinse cells EDTA or EGTA thoroughly before using.
Page 301
• Use dedicated plasticware for this analysis. Plastic sample cells must be used. Glass will contaminate the sample. Multi-pathlength Cell Method 8374 Hach Programs Touch Install the cell and cell Rinse a plastic Fill the plastic...
Page 302
Hardness, Total Zero Add the contents of Cap the cell and swirl Install the Touch Zero one Chlorophosphonazo to mix. (This is the blank.) multi-pathlength cell The display will show: Solution Pillow to the adapter. Use the 25-mm 0 µg/L CaCO sample cell.
Page 303
Hardness, Total Interferences Interference studies were conducted at various hardness levels between 0 and 500 µg/L as CaCO . Various cations and anions were evaluated at levels in the range appropriate to ultra pure water applications. An ion is said to interfere when the resulting concentration is changed by ±10%.
Page 304
Hardness, Total Accuracy Check Standard Additions Method (Sample Spike) 1. Touch . Touch . A summary of the standard Options Standard Additions additions procedure will appear. 2. Touch Change the sample volume to read 25 mL. Change the Standard Edit. Addition increments to 0.1 mL, 0.2 mL, and 0.3 mL.
Page 305
Hardness, Total Summary of Method Calcium and magnesium combine equivalently with the Chlorophosphonazo Indicator to form a colored complex which absorbs light very strongly at 669 nm. One drop of the CDTA reagent breaks up this complex, and the resultant decrease in color is proportional to the amount of calcium and magnesium (as CaCO ) in the sample.
Page 307
• Use dedicated plastic ware for this analysis. • Install the Pour-Thru Cell into the adapter so that the long pathlength (1-in./25-mm) is parallel to the front of the instrument. DR/2400 Pour-Thru Cell Method 8374 Hach Programs Touch Install the Pour-Thru Fill a clean, 125-mL...
Page 308
Hardness, Total Fill this rinsed Pour the contents of Add 2.0 mL of Pour approximately cylinder to the 50-mL the 50-mL cylinder back Chlorophosphonazo half (25 mL) of the mark with sample from into the flask. Reagent to the sample sample into the the flask.
Page 309
Hardness, Total Flush the Pour-Thru cell with an additional 50-mL of ultra-pure water. Interferences Interference studies were conducted at various hardness levels between 0 and 500 µg/L as CaCO . Various cations and anions were evaluated at levels in the range appropriate to ultra pure water applications.
Page 310
Hardness, Total Treating Analysis Labware Clean all containers used in this test thoroughly to remove any traces of calcium or magnesium. If possible, use plastic containers for all analysis and storage. Clean containers by normal means, then rinse with ultra-pure (aldehyde-free) water.
Page 311
Hardness, Total 6. After completing the sequence, touch to view the best-fit line through Graph the standard additions data points, accounting for matrix interferences. Touch , then select and touch to view the relationship between View: Fit Ideal Line the sample spikes and the “Ideal Line” of 100% recovery. See Section 3.2.2 Standard Additions on page 32 for more information.
Page 313
• The final samples will have a pH less than 2, which is considered corrosive (0002) by the Federal RCRA. Reagent Solution Method 8141 Hach Programs 10 mL 10 mL 10 mL 10 mL...
Page 314
Read Complete steps 6–8 Results will appear in µg/ during this period. AccuVac Ampul Method 8141 Hach Programs Keep the tips immersed while the ampules fill completely. Touch Collect at least 40 mL Fill a HydraVer Immediately touch of sample in a 50-mL Hydrazine AccuVac®...
Page 315
Hydrazine Zero Read Place the blank into Touch After the timer beeps, Immediately after Zero the cell holder. place the prepared the timer beeps, touch The display will show: sample in the cell holder. . Results will appear Read 0 µg/L N in µg/L N Interferences Interfering Substance...
Page 317
• Wipe the outside of sample cells before each insertion into the instrument cell holder. Use a damp towel followed by a dry one to remove fingerprints or other marks. Powder Pillows Method 8031 Hach Programs Touch Fill a cell with 10 mL Add the contents of Touch the timer icon.
Page 318
Wipe the blank and place the cell holder. it into the cell holder. Close the cover. AccuVac Ampul Method 8031 Hach Programs Hach Programs Touch Fill a sample cell with Fill a DPD Total Quickly invert the 10 mL of sample. (This is...
Page 319
Iodine Zero 10 mL Touch the timer icon. Wipe the blank and Touch Within three minutes Zero place it into the cell after the timer beeps, Touch The display will show: holder. wipe the prepared A three-minute reaction 0.00 mg/L I sample and place it into period will begin.
Page 321
• Use clean clippers, free of rust, and wipe with a dry towel. Do not allow clippers to contact contents of the pillow. • FerroZine Iron Reagent may crystallize or precipitate when exposed to cold temperatures during shipment. Reagent quality is not affected. Place the reagent in warm water to redissolve. Method 8147 Hach Programs 25 mL 25 mL 20 mL...
Page 322
Iron 25 mL 25 mL 20 mL 20 mL Zero 25 mL 20 mL 10 mL 10 mL 10 mL Fill another sample When the timer Touch Place the prepared Zero cell with 25 mL of sample beeps, insert the blank sample into the cell The display will show: (this is the blank).
Page 323
Iron Sample Collection, Storage and Preservation Collect samples in acid-washed glass or plastic bottles. To preserve samples, adjust the sample pH to 2 or less with concentrated Nitric Acid, ACS (Cat. No. 152-49) (about 2 mL per liter). Samples preserved in this manner can be stored up to six months at room temperature.
Page 325
• Underrange appears on the display when the instrument is zeroed or when the determined sample concentration is below the operating range listed for this method. UniCell Vials Hach Programs Touch Pipet 4 mL of sample Cap and invert the Touch the timer icon.
Page 326
Iron Zero Read Install the 16-mm cell Touch Wipe the sample vial Touch Zero Read adapter. and place the prepared The display will show: Results will appear in sample into the cell Note: See Section 2.6 Sample mg/L Free Fe. 0.00 mg/L Free Fe holder.
Page 327
Iron Accuracy Check Standard Additions Method (Sample Spike) 1. After reading test results, leave the sample cell (unspiked sample) in the instrument. 2. Touch . Touch . A summary of the standard Options Standard Additions additions procedure will appear. 3. Touch to accept the default values for standard concentration, sample volume, and spike volumes.
Page 329
Place the reagent in warm water to re-dissolve. • Install the Pour-Thru Cell into the adapter so that the long pathlength (1-in./25-mm) is parallel to the front of the instrument. Pour-Thru Cell Method 8147 Hach Programs Touch Install the Pour-Thru Rinse two clean...
Page 330
Iron Fill the rinsed Pour the contents of Add 1.0 mL of Touch the timer icon. cylinder to the 50-mL the 50-mL cylinder into FerroZine Iron Reagent Touch mark with sample. one of the flasks. Measure Solution to one of the A five-minute reaction a second 50 mL portion of flasks using the Repipet...
Page 331
Iron (continued) Interfering Substance Interference Levels 1. Fill a 50-mL graduated cylinder with 50 mL of sample. 2. Transfer the sample into a clean glass 125-mL Erlenmeyer flask. 3. Add 1.0-mL of FerroZine Iron Reagent Solution Cat. No. 2301-53) and swirl to mix. 4.
Page 333
See the instrument manual for more information on Running a Reagent Blank. • If ferrous iron is present, an orange color will form after adding the reagent. Powder Pillows Method 8146 Hach Programs 25 mL 25 mL 20 mL 20 mL...
Page 334
0.00 mg/L Fe Touch Read Results will appear in mg/L Fe AccuVac Ampul Method 8146 Hach Programs 25 mL 20 mL 10 mL Touch Fill a sample cell with Fill a Ferrous Iron Quickly invert the 25 mL of sample (the AccuVac®...
Page 335
Iron, Ferrous 25 mL 20 mL Zero 10 mL Touch the timer icon. When the timer Touch Place the AccuVac Zero beeps, place the blank Ampul into the cell Touch The display will show: into the cell holder. holder. A three-minute reaction 0.00 mg/L Fe Touch Read...
Page 337
** Federal Register, June 27, 1980; 45 (126:43459) Tips and Techniques • Digestion is required for determining total iron for EPA reporting purposes. See the Hach Water Analysis Handbook for digestion procedures. • For more accurate results, determine a reagent blank value for each new lot of reagent. Follow the procedure using deionized water in place of the sample.
Page 338
0.00 mg/L Fe Touch Read Results will appear in mg/L Fe. AccuVac Ampul Method 8008 Hach Programs 25 mL 20 mL 10 mL Touch Fill a sample cell with Fill a FerroVer Iron Quickly invert the 25 mL of sample. Collect AccuVac®...
Page 339
Iron, Total 25 mL 20 mL Zero 10 mL Touch the timer icon. When the timer Touch Place the AccuVac Zero beeps, place the blank Ampul into the cell Touch The display will show: into the cell holder. holder. A three-minute reaction 0.00 mg/L Fe Touch Read...
Page 340
Iron, Total Sample Collection, Storage and Preservation 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 concentrated nitric acid (about 2 mL per liter) (Cat.
Page 341
Iron, Total 3. Touch . Touch to accept the displayed concentration. If an alternate Adjust concentration is used, touch the number in the box to enter the actual concentration, then touch . Touch Adjust See Section 3.2.4 Adjusting the Standard Curve on page 40 for more information. Method Performance Precision Standard: 1.000 mg/L Fe...
Page 343
Tips and Techniques • Digestion is required for determining total iron. See the Hach Water Analysis Handbook for digestion procedures. • For more accurate results, determine a reagent blank value for each new lot of reagent. Follow the procedure using deionized water in place of the sample.
Page 344
Read and shake for 30 seconds. Results will appear in mg/L Fe. ® TPTZ AccuVac Ampul Method 8112 Hach Programs 25 mL 20 mL 10 mL Touch Collect at least 40 mL Fill a TPTZ Iron Invert the ampule ®...
Page 345
Iron, Total 25 mL 20 mL Zero 10 mL Touch the timer icon. When the timer Touch Place the prepared Zero beeps, place the blank sample into the adapter. Touch The display will show: into the adapter. Touch Read A three-minute reaction 0.000 mg/L Fe period will begin.
Page 346
Iron, Total Sample Collection, Storage and Preservation Collect samples in acid-washed glass or plastic bottles. To preserve samples, adjust the sample pH to 2 or less with about 2 mL/L Nitric Acid, ACS (Cat. No. 152-49). Store preserved samples up to six months at room temperature.
Page 347
Iron, Total 3. Touch . Touch to accept the displayed concentration. If an alternate Adjust concentration is used, touch the number in the box to enter the actual concentration, then touch . Touch Adjust See Section 3.2.4 Adjusting the Standard Curve on page 40 for more information. Method Performance Precision Standard: 1.000 mg/L Fe...
Page 349
Tips and Techniques • Digestion is required for total iron determination. See the Hach Water Analysis Handbook for digestion procedures. • Rinse glassware with a 1:1 hydrochloric acid solution. Rinse again with deionized water. These two steps will remove iron deposits that can cause slightly high results.
Page 350
Iron, Total 25 mL 25 mL 25 mL 20 mL 20 mL 20 mL 10 mL 10 mL 10 mL Fill a clean, round Add the contents of Touch the timer icon. Fill a second round sample cell to the 25-mL one FerroMo Iron sample cell with the Touch...
Page 351
Iron, Total Sample Collection, Storage and Preservation Collect samples in acid-washed glass or plastic bottles. To preserve samples, adjust the sample pH to 2 or less with hydrochloric acid (about 2 mL per liter) (Cat. No. 134-49). Samples preserved in this manner can be stored up to six months at room temperature.
Page 353
• The sampling requirements for “first-draw” analysis are detailed in Sample Collection, Storage and Preservation on page 4. • Reagents will stain the sample cells, rinse the cells with 1:1 HNO , followed by deionized water. Fast Column Extraction Method 8317 Hach Programs Touch Fill a 100-mL plastic Using a plastic 1-mL Touch the timer icon.
Page 354
Lead When the timer Mount a new Fast Soak the cotton plug Pour the prepared beeps, use a second 1-mL Column Extractor in a with deionized water and sample slowly into the plastic dropper to add ring stand with a clamp. compress it with the center of the Column 2.0 mL of pPb-2 Fixer...
Page 355
Lead 25 mL 20 mL Zero 25 mL 20 mL 10 mL 10 mL Add the contents of Touch the timer icon. When the timer Touch Zero one pPb-5 Indicator beeps, place the sample Touch The display will show: Powder Pillow to the cell into the cell holder.
Page 356
Lead The Extractor plunger may be reused for more than one test but should be rinsed between uses. Interfering Substance Interference Levels and Treatments Aluminum, Al 0.5 mg/L Ammonium, NH 500 mg/L Barium, Ba 6 mg/L Calcium, Ca 500 mg/L Chloride, Cl –...
Page 357
Lead Sampling for Lead Contamination in Household Pipes for Point-of-use Drinking Water • The sample should be collected after sitting in pipes with no flow for 8 to 18 hours. • Add 10 mL of pPb-1 Acid Preservative (Cat. No. 23685-31) to a one-liter bottle.
Page 358
Lead 4. Open a container of 10-mg/L (10,000 µg/L) Lead Standard Solution. 5. Prepare three sample spikes. Fill three beakers with 100 mL of sample. Use ® the TenSette Pipet to add 0.1 mL, 0.2 mL, and 0.3 mL of standard, respectively, to each sample and mix thoroughly.
Page 359
Lead Method Performance Precision Standard: 750.0 µg/L Pb Program Standard Deviation of 7 Replicate Standards 10.15 µg/L Pb See Section 3.4.3 Precision on page 44 for more information, or if the standard concentration did not fall within the specified range. Sensitivity ∆Abs ∆Concentration...
Page 361
• Underrange appears on the display when the instrument is zeroed or when the determined sample concentration is below the operating range listed for this method. UniCell Vials Hach Programs Touch Pipet 10.0 mL of Use the spoon to add...
Page 362
Lead Zero Touch the timer icon. Install the 16-mm cell Touch Pipet 0.3 mL of Zero adapter. Masking Solution C Touch The display will show: (HCT 152 C) into the Note: See Section 2.6 Sample A second two-minute 0.00 mg/L Free Pb sample vial.
Page 363
Lead Total lead, including undissolved lead hydroxide and complexed lead, can only be determined after digesting with the Metal Prep Set, HCT 200. Note: The total lead measuring range is 0.24–2.40 mg/L. Sample Collection, Storage and Preservation Collect samples in acid-cleaned glass or plastic containers. No acid addition is necessary if analyzing the samples immediately.
Page 365
Subtract the reagent blank value from the final results or perform a reagent blank adjust See the instrument manual for more information on Running a Reagent Blank. Powder Pillows Method 8034 Hach Programs Touch Fill a round sample Add the contents of Add the contents of...
Page 366
Manganese Zero 10 mL Touch the timer icon. Fill another round When the timer Touch Zero sample cell with 10 mL of beeps, place the blank Touch The display will show: sample. into the cell holder. A two-minute reaction 0.0 mg/L Mn period will begin.
Page 367
Manganese Sample Collection, Storage and Preservation Collect samples in acid-washed plastic bottles. Do not use glass containers due to possible adsorption of Mn to glass. If samples are acidified, adjust the pH to 4–5 with 5.0 N Sodium Hydroxide (Cat. No. 2450-32) before analysis. Do not exceed pH 5, as manganese may precipitate.
Page 369
>11 to prevent release of hydrogen cyanide gas. See Section Section 4 Waste Management and Safety on page 55 for more information on proper disposal of these materials. Powder Pillows Method 8149 Hach Programs 10 mL 10 mL Touch Pour 10.0 mL of...
Page 370
Manganese 10 mL Add 15 drops of Add 21 drops of PAN Touch the timer icon. When the timer Alkaline-Cyanide Indicator Solution, 0.1%, beeps, wipe the blank Touch Reagent Solution to each to each sample cell. Cap and place it into the cell A two-minute reaction cell.
Page 371
Manganese For samples that contain hardness greater than 300 mg/L CaCO , add 10 drops of Rochelle Salt Solution (Cat. No. 1725-33) to the sample after adding the Ascorbic Acid Powder Pillow in step 4. Sample Collection, Storage and Preservation Collect samples in a clean plastic container.
Page 373
DR/2400 Mercury Cold Vapor Mercury Concentration Method* Method 10065 (0.1 to 2.5 µg/L) Scope and Application: For water, wastewater, and seawater * Patent no. 5,733,786 Tips and Techniques • Perform phase 1 of the procedure in a fume hood. Toxic chlorine or other gases may be produced. •...
Page 374
Mercury Add 7.5 g of Cover the flask with a Continue to stir and Cool the digested potassium permanganate watch glass. Begin heat the sample at 90 °C sample to room to the sample. Stir until heating the sample to a for two hours.
Page 375
Mercury Return the cool, Using a 0.5-g Remove the stir bar. The digested sample digested sample to the measuring spoon, add is now ready for cool, magnetic stirring 0.5 g additions of processing by cold vapor hot plate. Turn on the hydroxylamine- separation and stirrer.
Page 376
Mercury Connect the power to Disconnect the Remove the 100-mL Pipet 2 mL of HgEx the vacuum pump and vacuum using the quick Erlenmeyer flask from Reagent C into the apply vacuum to the disconnect when the Mercury Absorber Mercury Absorber Mercury Absorber HgEx Reagent B begins Column.
Page 377
Mercury Hach Programs Touch Touch the timer icon. After the timer beeps, Pipet 8 mL of HgEx Touch remove the glass elbow Reagent B into the Hach Programs from the top of the Mercury Absorber A five-minute reaction Select program...
Page 378
Mercury Turn off, or Remove the distilling Pipet 3 mL of HgEx disconnect power to the Receiver from the Reagent B into the vacuum pump when the Mercury Absorber Mercury Absorber volume in the Distilling Column. Reconnect the Column without Receiver reaches the 100-mL Erlenmeyer flask applying vacuum.
Page 379
Mercury Zero 10 mL 10 mL During the reaction After the timer beeps, Touch Remove the cell from Zero period, transfer the place the prepared the cell holder. Add the The display will show: solution to a sample cell. sample into the cell contents of one HgEx 0.1 µg/L Hg Wipe the sample cell...
Page 380
Mercury Ion or Substance Concentration 7 mg/L Ag 10 mg/L Al 500 µg/L Au 10 mg/ L Cd 10 mg/L Co 10 mg/L Cr 10 mg/L Cu – – 1.0 mg/L F 100 mg/L Fe 1 µg/L Hg 10 mg/L Mo 10 mg/L Ni –...
Page 381
6. Test the eluate as described in Phase 3. The displayed concentration should be 0.9–1.1 µg/L Hg. System Start Up Hach recommends that the analyst perform a few analyses on mercury standards and blanks for system equilibration before beginning sample testing. This allows the system to stabilize before processing samples.
Page 382
Gas Washing Bottle with the glass elbow as in the procedure. Glassware Care Hach recommends using dedicated glassware and sample cells because of the sensitivity of this procedure. Thoroughly clean the glassware and sample cells between tests. After washing, rinse with 1:1 hydrochloric acid solution, then rinse several times with deionized water.
Page 383
Pollution Prevention and Waste Management Proper management and disposal of waste is the responsibility of the waste generator. Hach Company provides waste disposal information as a guideline only. It is up to the generator to arrange for proper disposal and comply with applicable local, state, and federal regulations governing waste disposal.
Page 385
• Twenty Antibody Cuvettes are provided with each reagent set. One Antibody Cuvette will be used for each calibrator and each sample. Cuvettes are not reusable. • Hach Company recommends wearing protective nitrile gloves for this procedure. Metolachlor Page 1 of 8...
Page 386
Metolachlor Immunoassay Procedure for Water λ Touch Label an Antibody Place the cuvettes Pipet 0.5 mL of each Cuvette for each into the rack snugly. calibrator into the Single Wavelength calibrator and each appropriately labeled λ then touch the button. sample to be tested.
Page 387
Metolachlor At the end of the Wash each cuvette 20-minute period, discard forcefully and thoroughly the contents of all the four times with deionized cuvettes into an water. Empty the rinse appropriate waste water into the waste container. container. Note: Ensure most of the water is drained from the cuvettes by turning the cuvettes upside down and tapping them lightly...
Page 388
Metolachlor Measuring the Color Zero Label and fill a Install the 1-cm Touch Place the first Zero Zeroing Cuvette with square cell adapter. calibrator into the The display will show: deionized water. Wipe celladapter. Note: See Section 2.6 Sample 0.000 Abs the outside of all the Cell Adapters in the Instrument Touch...
Page 389
Metolachlor Using the 1-cm MicroCuvette Rack This rack (see Figure 1) has been designed specifically to aid in achieving precise and accurate results when using the immunoassay technique to analyze several samples at the same time. Figure 1 The 1-cm MicroCuvette Rack Loading the Rack —...
Page 390
Metolachlor Interpretation Sample #1 — Sample reading is less than the readings for both calibrators. Therefore the sample concentration of Metolachlor is greater than both 0.5 ppb and 2.0 ppb Metolachlor. Sample #2 — Sample reading is between the readings for the 0.5 ppb and 2.0 ppb Metolachlor calibrators.
Page 391
Rack, for 1-cm Micro Cuvettes..................each....48799-00 Wipes, disposable ....................... box .....20970-00 ® TenSette , Pipet, 0.1–1.0 mL....................each....19700-01 Tips, for pipettor 19700-01....................1000/pkg...21856-28 * Immunoassay components are manufactured for Hach Company by Beacon Analytical Systems, Inc. Metolachlor Page 7 of 8 MET_None_Other_IMM_Eng_Ody.fm...
Page 393
• Filter turbid samples using filter paper (Cat. No. 1894-57) and a funnel (Cat. No. 1083-67). • After all reagents have been added, the presence of molybdenum will cause a yellow color to form. Powder Pillows Method 8036 Hach Programs Touch Fill a sample cell with Add the contents of Add the contents of ®...
Page 394
Molybdenum, Molybdate 10 mL Add the contents of Touch the timer icon. When the timer Insert the blank into one MolyVer 3 Reagent beeps, fill a second cell the cell holder. Touch Powder Pillow. Swirl to with 10 mL of the original A five-minute reaction mix (the prepared sample (the blank).
Page 395
Molybdenum, Molybdate AccuVac Ampul Method 8036 Hach Programs Touch Fill a sample cell with Add four drops of Fill a MolyVer 6 ® 10 mL of sample (the 0.4 M CDTA Standard AccuVac Ampul with Hach Programs blank). Solution to the sample in the treated sample.
Page 396
Molybdenum, Molybdate Read Place the prepared Touch Read sample into the cell Results will appear in holder. mg/L Mo Interferences Interfering Substance Interference Levels and Treatments Aluminum Greater than 50 mg/L Chromium Greater than 1000 mg/L Samples containing 10 mg/L copper or more will exhibit an increasing positive interference upon Copper standing.
Page 397
Molybdenum, Molybdate 5. Prepare three sample spikes. Fill three Mixing Cylinders (Cat. No. 1896-40) ® with 30 mL of sample. Use the TenSette Pipet to add 0.2 mL, 0.4 mL, and 0.6 mL of standard, respectively, to each sample and mix thoroughly. Note: For AccuVac Ampuls, fill three Mixing Cylinders (Cat.
Page 399
• Wipe the outside of sample cells before each insertion into the instrument cell holder. Use a damp towel followed by a dry one to remove fingerprints or other marks. • Filter turbid samples using filter paper (Cat. No. 1894-57) and a funnel (Cat. No. 1083-67). Powder Pillows Method 8169 Hach Programs Touch Fill a 25-mL Add the contents of Stopper the cylinder...
Page 400
Molybdenum, Molybdate Zero Read 10 mL 10 mL Wipe the blank and Touch Wipe the developed Touch Zero Read place it into the cell sample and place it into The display will show: Results will appear in holder. the cell holder. mg/L Mo 0.00 mg/L Mo Interferences...
Page 401
Molybdenum, Molybdate Table 1 Substances that Cause a Negative Interference (continued) Interfering Substance Interference Levels and Treatments Sulfite Greater than 6500 mg/L * Read the molybdenum concentration immediately after the beep of the 2-minute reaction period. Table 2 Substances that Cause a Positive Interference Interfering Substance Interference Levels and Treatments Benzotriazole...
Page 402
Molybdenum, Molybdate Sample Collection, Storage and Preservation Collect samples in glass or plastic bottles. Analyze samples immediately. Accuracy Check Standard Additions Method (Sample Spike) 1. After reading test results, leave the sample cell (unspiked sample) in the instrument. Verify the chemical form. 2.
Page 403
Molybdenum, Molybdate Method Performance Precision Standard: 2.00 mg/L Mo Program 95% Confidence Limits of Distribution 1.93–2.07 mg/L Mo See Section 3.4.3 Precision on page 44 for more information, or if the standard concentration did not fall within the specified range. Sensitivity ∆Abs ∆Concentration...
Page 405
• Wipe the outside of sample cells before each insertion into the instrument cell holder. Use a damp towel followed by a dry one to remove fingerprints or other marks. Powder Pillows Method 8037 Hach Programs Touch Measure 300 mL of Add the contents of Touch the timer icon.
Page 406
Nickel HRS MIN SEC HRS MIN SEC When the timer Touch the timer icon. When the timer Close the stopcock beeps, add the contents of beeps, add 10 mL of and invert for 30 seconds. Touch one Nickel 2 Reagent chloroform.
Page 407
Nickel 25 mL 25 mL 20 mL 20 mL Zero 25 mL 20 mL 10 mL 10 mL 10 mL Fill a second cell with Wipe the blank and Touch Wipe the prepared Zero 25 mL of chloroform. place it into the cell sample and place it into The display will show: (This is the blank.)
Page 408
Nickel Accuracy Check Standard Additions Method (Sample Spike) 1. After reading test results, leave the sample cell (unspiked sample) in the instrument. 2. Touch . Touch . A summary of the standard Options Standard Additions additions procedure will appear. 3. Touch to accept the default values for standard concentration, sample volume, and spike volumes.
Page 409
Nickel Method Performance Precision Standard: 1.00 mg/L Ni Program 95% Confidence Limits of Distribution 0.93–1.07 mg/L Ni See Section 3.4.3 Precision on page 44 for more information, or if the standard concentration did not fall within the specified range. Sensitivity ∆Abs ∆Concentration Portion of Curve...
Page 411
• Wipe the outside of sample cells before each insertion into the instrument cell holder. Use a damp towel followed by a dry one to remove fingerprints or other marks. Powder Pillows Method 8150 Hach Programs 10 mL 10 mL 10 mL...
Page 412
Nickel 10 mL 10 mL 10 mL 10 mL 10 mL Using the plastic Touch the timer icon. When the timer Wipe the blank and dropper provided, add beeps, add the contents of place it into the cell Touch 0.5 mL of 0.3% PAN one EDTA Reagent holder.
Page 413
Nickel Interferences Interfering Substance Interference Levels and Treatments 32 mg/L 1000 mg/L as (CaCO 20 mg/L – 8000 mg/L Interfere at all levels. Use either the Digesdahl or vigorous digestion to eliminate this interference Chelating agents (see Section 2). 20 mg/L 40 mg/L 15 mg/L –...
Page 414
Nickel ® 4. Snap the neck off a Nickel Voluette Ampule Standard, 50-mg/L Ni. 5. Prepare three sample spikes. Fill three Mixing Cylinders (Cat. No. 1896-40) ® with 25 mL of sample. Use the TenSette Pipet to add 0.1 mL, 0.2 mL, and 0.3 mL of standard, respectively, to each sample and mix thoroughly.
Page 415
Nickel Summary of Method After buffering the sample and masking any Fe with pyrophosphate, the nickel is reacted with 1-(2-Pyridylazo)-2-Naphthol indicator. The indicator forms complexes with most metals present. After color development, EDTA is added to destroy all metal-PAN complexes except nickel and cobalt. The instrument automatically adjusts for cobalt interference by measuring the absorbance of the sample at both 560 nm and 620 nm.
Page 417
• The temperature of the water sample and the sample vial should be between 15–25 °C (59–77 °F). • Underrange appears on the display when the instrument is zeroed or when the determined sample concentration is below the operating range listed for this method. UniCell Vials Hach Programs Touch Pipet 4.0 mL of Pipet 0.4 mL of...
Page 418
Nickel Zero Touch the timer icon. Install the 16-mm cell Touch Wipe the sample vial Zero adapter. and place the prepared Touch The display will show: sample into the Note: See Section 2.6 Sample A 3-minute reaction 0.00 mg/L Free Ni celladapter.
Page 419
Nickel Accuracy Check Standard Additions Method (Sample Spike) 1. After reading test results, leave the sample cell (unspiked sample) in the instrument. 2. Touch . Touch . A summary of the standard Options Standard Additions additions procedure will appear. 3. Touch to accept the default values for standard concentration, sample volume, and spike volumes.
Page 421
Federal, State and local hazardous waste regulations. For information on pollution prevention and waste management, refer to Section 4 on page 55. Powder Pillows Method 8039 Hach Programs Touch Fill a round sample Add the contents of Touch the timer icon.
Page 422
Nitrate Zero 10 mL When the timer When the timer Wipe the blank and Touch Zero beeps, touch the timer beeps, fill a second round place it into the cell The display will show: icon. Touch sample cell with 10 mL of holder.
Page 423
Nitrate ® AccuVac Ampul Method 8039 Hach Programs Hach Programs Touch Collect at least 40 mL Fill a NitraVer 5 Touch the timer icon. ® of sample in a 50-mL Nitrate AccuVac Ampul Touch Hach Programs beaker. with sample. Keep the tip...
Page 424
Nitrate Read Within one minute Touch Read after the timer beeps, Results will appear in wipe the ampule and – mg/L NO –N. place into the cell holder. Interferences Interfering Substance Interference Levels and Treatments Chloride concentrations above 100 mg/L will cause low results. The test may be used at high Chloride chloride concentrations (seawater) but a calibration must be done using standards spiked to the same chloride concentration.
Page 425
Nitrate Accuracy Check Standard Additions Method (Sample Spike) 1. After reading test results, leave the sample cell (unspiked sample) in the instrument. Verify the chemical form. 2. Touch . Touch . A summary of the standard Options Standard Additions additions procedure will appear. 3.
Page 427
• Prepared samples will contain cadmium and must be disposed of according to Federal, State and local hazardous waste regulations. For information on pollution prevention and waste management, refer to Section 4. Powder Pillows Method 8171 Hach Programs Hach Programs Touch Fill a round sample Add the contents of Touch the timer icon.
Page 428
Nitrate Zero 10 mL When the timer When the timer Place the blank into Touch Zero beeps, touch the timer beeps, fill a second round the cell holder. The display will show: icon. Touch sample cell with 10 mL of –...
Page 429
Nitrate ® AccuVac Ampul Method 8171 Hach Programs Touch Collect at least 40 mL Fill a NitraVer 5 Touch the timer icon. ® of sample in a 50-mL Nitrate AccuVac Ampul Touch Hach Programs beaker. with sample. Keep the tip...
Page 430
Nitrate Read Within two minutes Touch Read after the timer beeps, Results will appear in wipe the ampule and – mg/L NO –N. place it into the cell holder. Interferences Interfering Interference Levels and Treatments Substance Chloride concentrations above 100 mg/L will cause low results. The test may be used at high chloride Chloride concentrations (seawater) but a calibration must be done using standards spiked to the same chloride concentration.
Page 431
Nitrate Before analysis, warm the sample to room temperature and adjust the pH to 7 with 5.0 N Sodium Hydroxide Standard Solution (Cat. No. 2450-53). Do not use mercury compounds as preservatives. Correct the test result for volume additions by dividing the total volume (acid + base + sample) by the original sample volume and multiplying the test result by this factor.
Page 433
• Shaking time and technique influence color development. Analyze a standard solution several times and adjust the shaking time to obtain the correct result. Use this time for analyzing samples Powder Pillows Method 8192 Hach Programs Touch Fill a 25-mL Add the contents of Touch the timer icon.
Page 434
Nitrate 10 mL When the timer When the timer Add the contents of Touch the timer icon. beeps, touch the timer beeps, carefully pour one NitriVer3 Nitrite Touch icon again. 10 mL of the sample into Reagent Powder Pillow Shake the sample cell a clean, round sample to the sample cell (this is Touch...
Page 435
Nitrate Read 10 mL Place the prepared Touch Read sample into the cell Results will appear in holder. – mg/L NO –N. Interferences Interfering Substance Interference Levels and Treatments Calcium 100 mg/L Chloride concentrations above 100 mg/L will cause low results. The test may be used at high Chloride chloride concentrations (seawater) but a calibration must be done using standards spiked to the same chloride concentration.
Page 436
Nitrate Accuracy Check Standard Additions Method (Sample Spike) 1. After reading test results, leave the sample cell (unspiked sample) in the instrument. Verify the chemical form. 2. Touch . Touch . A summary of the standard Options Standard Additions additions procedure will appear. 3.
Page 437
Nitrate Method Performance Precision – Standard: 0.2 mg/L NO –N Program 95% Confidence Limits of Distribution – 0.18–0.23 mg/L NO –N See Section 3.4.3 Precision on page 44 for more information, or if the standard concentration did not fall within the specified range. Sensitivity ∆Abs ∆Concentration...
Page 439
• Wipe the outside of sample cells before each insertion into the instrument cell holder. Use a damp towel followed by a dry one to remove fingerprints or other marks. Test ‘N Tube Method 10020 Hach Programs Touch Remove the cap from Cap the tube and...
Page 440
A positive interference at concentrations greater than 12 mg/L. Remove nitrite interference up to Nitrite 100 mg/L by adding 400 mg (one full 0.5 g Hach measuring spoon) of Urea (Cat. No. 11237-26) to 10 mL of sample. Swirl to dissolve. Proceed with the nitrate test as usual.
Page 441
Nitrate Sample Collection, Preservation, and Storage Collect samples in clean plastic or glass bottles. Store at 4 °C (39 °F) or lower if the sample is to be analyzed within 24 to 48 hours. Warm to room temperature before running the test. For longer storage periods (up to 14 days), adjust sample pH to 2 or less with Concentrated Sulfuric Acid, ACS (about 2 mL per liter) (Cat.
Page 443
• Make sure that the temperature of the sample and the reagents is between 20 and 24 °C. Higher temperatures can cause high-bias results; lower temperatures can cause low-bias results. UniCell Vials Hach Programs Touch Pipet 0.2 mL of Cap the vial and...
Page 444
Nitrate Zero HRS MIN SEC HRS MIN SEC Cap the sample vial Touch the timer icon. Install the 16-mm cell Touch Zero and invert a few times adapter. Touch The display will show: until the reagents are Note: See Section 2.6 Sample A 15-minute reaction 0.0 mg/L NO mixed and appear...
Page 445
Nitrate No interference up to: , Zn , Ni , Hg , Fe , Cd , Sn 50 mg/L , Cu , Fe 10 mg/L 5 mg/L – 2 mg/L Interfering Substance Interferes above: 200 mg/L (high bias) Nitrite 2 mg/L (high bias) Chloride 500 mg/L (low bias) Sample Collection, Preservation, and Storage...
Page 447
• Wipe the outside of sample cells before each insertion into the instrument cell holder. Use a damp towel followed by a dry one to remove fingerprints or other marks. Powder Pillows Method 8507 Hach Programs Touch Fill a round sample Add the contents of Touch the timer icon.
Page 448
Results will appear in – mg/L NO –N. ® AccuVac Ampul Method 8507 Hach Programs Touch Pour at least 40 mL of Fill a NitriVer 3 Invert the ampule ® sample into a 50-mL Nitrite AccuVac Ampul several times to mix.
Page 449
Nitrite Zero 10 mL Touch the timer icon. When the timer Wipe the blank and Touch Zero beeps, fill a sample cell place it into the cell Touch The display will show: with at least 10 mL of holder. – A 20-minute reaction 0.000 mg/L NO –N...
Page 450
Accuracy Check Standard Solution Method Preparing nitrite standards is difficult. A standard should be prepared by a trained chemist. Hach recommends using the standard preparation instructions in Standard Methods for the Examination of Water and Wastewater, Method 4500—NO -B (p. 4–86 of 18th edition). Prepare a 0.150-mg/L standard.
Page 451
Nitrite Sensitivity ∆Abs ∆Concentration Program Portion of Curve – Entire range 0.010 0.002 mg/L NO –N – Entire range 0.010 0.002 mg/L NO –N See Section 3.4.5 Sensitivity on page 44 for more information. Summary of Method Nitrite in the sample reacts with sulfanilic acid to form an intermediate diazonium salt.
Page 453
• Wipe the outside of sample cells before each insertion into the instrument cell holder. Use a damp towel followed by a dry one to remove fingerprints or other marks. Powder Pillows Method 8153 Hach Programs Touch Fill a round sample Add the contents of Touch the timer icon.
Page 454
Nitrite Zero 10 mL Fill another sample Wipe the blank and Touch After the timer beeps, Zero cell with 10 mL of sample place it into the cell gently invert the The display will show: (this is the blank). holder. prepared sample twice.
Page 455
Standard Solution Method Preparing nitrite standards is difficult. A standard should be prepared by a trained chemist. Hach recommends using the standard preparation instructions in Standard Methods for the Examination of Water and Wastewater. Prepare a 200-mg/L standard using Sodium Nitrite, ACS (Cat. No. 2452-01).
Page 457
• Wipe the outside of sample cells before each insertion into the instrument cell holder. Use a damp towel followed by a dry one to remove fingerprints or other marks. Test ‘N Tube Method 10019 Hach Programs Touch Fill a Test ‘N Tube Cap and shake to Touch the timer icon.
Page 458
Nitrite Zero When the timer beeps, Install the 16-mm Touch Place the prepared Zero fill an empty Test ‘N adapter. sample cell into the cell The display will show: Tube™ vial with 5 mL of holder. Note: See Section 2.6 in the –...
Page 459
Standard Solution Method Preparing nitrite standards is difficult. A standard should be prepared by a trained chemist. Hach recommends using the standard preparation instructions in Standard Methods for the Examination of Water and Wastewater, 18th ed., under the headings “Stock nitrite solution,” “Intermediate nitrite solution,” and “Standard nitrite solution.”...
Page 461
• See 3.2.4 on page 40 for information on calibration curve adjustment. • Underrange appears on the display when the instrument is zeroed or when the determined sample concentration is below the operating range listed for this method. UniCell Vials Hach Programs Touch Pipet 4.0 mL of Immediately screw a Invert the sample vial sample into a sample vial.
Page 462
Nitrite Zero Touch the timer icon. Install the 16-mm cell Touch Wipe the sample vial Zero adapter. and place it into the A 10-minute reaction The display will show: celladapter. period will begin. Invert Note: See Section 2.6 Sample – 0.000 mg/L NO –N Cell Adapters in the Instrument...
Page 463
Nitrite Accuracy Check Standard Solution Method – Prepare a 0.25-mg/L NO –N standard solution by pipetting 1.00 mL of – 250-mg/L NO –N standard into a 1000-mL volumetric flask. Dilute to the mark with deionized water. Stopper and invert to mix. Prepare this solution daily. Perform the nitrite procedure as described.
Page 465
Flush with enough deionized water to dissolve. Rinse the cell thoroughly. • A yellow color will develop if ammonia is present. (The reagent will cause a faint yellow color in the blank.) Method 8038 Hach Programs Touch Fill a 25-mL mixing...
Page 466
Nitrogen, Ammonia 10 mL 10 mL Add three drops of Pipet 1.0 mL of Touch the timer icon. Pour each solution Polyvinyl Alcohol Nessler Reagent into each into a round sample cell. Touch Dispersing Agent to each cylinder. A one-minute reaction cylinder.
Page 467
Nitrogen, Ammonia Interferences Interfering Substance Interference Levels and Treatments Remove residual chlorine by adding 2 drops of sodium arsenite for each mg/L Cl from a 250 mL Chlorine sample. Sodium thiosulfate can be used in place of sodium arsenite. See Sample Collection, Storage, and Preservation below.
Page 468
1 N sodium hydroxide solution. Use a pH meter. 3. Set up the General Purpose Distillation Apparatus (Cat. No. 22653-00) as shown in the Hach Distillation Apparatus Manual. Pour the solution into the distillation flask. Add a stir bar. 4. Use a graduated cylinder to measure 25 mL of deionized water into a 250-mL Erlenmeyer flask.
Page 469
Nitrogen, Ammonia 5. Turn on the heater power switch. Set the stir control to 5 and the heat control to 10. Turn on the water and adjust to maintain a constant flow through the condenser. 6. Turn off the heater after collecting 150 mL of distillate. Immediately remove the collection flask to avoid sucking solution into the still.
Page 471
* Adapted from Clin. Chim. Acta., 14, 403 (1966) Tips and Techniques • A green color will develop if ammonia nitrogen is present. Powder Pillows Method 8155 Hach Programs Hach Programs 10 mL Touch Fill a round sample Fill another round...
Page 472
Less common interferences such as hydrazine and glycine will cause intensified colors in the prepared sample. Turbidity and color will give erroneous high values. Samples with severe Other Substances interferences require distillation. Hach recommends the distillation procedure using the Hach General Purpose Distillation Set (Cat. No. 22653-00). Sample Collection, Storage, and Preservation Collect samples in clean plastic or glass bottles.
Page 473
Nitrogen, Ammonia For longer storage, adjust the pH to 2 or less with concentrated (about 2 mL per liter) Sulfuric Acid (Cat. No. 979-49). Store samples at 4 °C or less. Samples preserved in this manner can be stored up to 28 days. Just before testing the stored sample, warm to room temperature and neutralize with 5.0 N Sodium Hydroxide Standard Solution (Cat.
Page 475
>11 to prevent release of hydrogen cyanide gas. See Section 4 on page 55 for further information in proper disposal of these materials. • A green color will develop if ammonia is present. Test ‘N Tube Method 10031 Hach Programs Touch Add 0.1 mL of sample Add 0.1 mL of Add the contents of to one AmVer™...
Page 476
Nitrogen, Ammonia Add the contents of Cap the vials tightly Touch the timer icon. Install the 16-mm one Ammonia Cyanurate and shake thoroughly to adapter. Touch Reagent Powder Pillow dissolve the powder. Note: See Section 2.6 in the A 20-minute reaction to each vial.
Page 477
Filter the sample through folded filter paper (Cat. No. 692-57). Use the solution in step 4. Give erroneous high values. Samples with severe interferences require distillation. Turbidity and color Hach recommends the distillation procedure using the Hach General Purpose Distillation Set (Cat. No. 22653-00). Sample Collection, Storage, and Preservation Collect samples in clean plastic or glass bottles.
Page 478
Nitrogen, Ammonia Accuracy Check Standard Additions Method (Sample Spike) 1. After reading test results, leave the sample cell (unspiked sample) in the instrument. 2. Touch . Touch . A summary of the standard Options Standard Additions additions procedure will appear. 3.
Page 479
Nitrogen, Ammonia Method Performance Precision Standard: 10.0 mg/L NH –N Program 95% Confidence Limits of Distribution 8.9–11.1 mg/L NH –N See Section 3.4.3 Precision on page 44 for more information, or if the standard concentration did not fall within the specified range. Sensitivity ∆Abs ∆Concentration...
Page 481
• Wipe the outside of sample cells before each insertion into the instrument cell holder. Use a damp towel followed by a dry one to remove fingerprints or other marks. • A green color will develop if ammonia is present. Test ‘N Tube Method 10023 Hach Programs Hach Programs Touch Add 2.0 mL of sample Add 2.0 mL of Add the contents of to one AmVer™...
Page 482
Nitrogen, Ammonia Add the contents of Cap the vials tightly Touch the timer icon. Install the 16-mm one Ammonia Cyanurate and shake thoroughly to adapter. Touch Reagent Powder Pillow dissolve the powder. Note: See Section 2.6 in the A 20-minute reaction to each vial.
Page 483
Less common interferences such as hydrazine and glycine will cause intensified colors in the prepared sample. Turbidity and color will give erroneous high values. Samples with severe Other interferences require distillation. Hach recommends the distillation procedure using the Hach General Purpose Distillation Set (Cat. No. 22653-00). Sample Collection, Storage, and Preservation Collect samples in clean plastic or glass bottles.
Page 484
Nitrogen, Ammonia 7. After completing the sequence, touch to view the best-fit line through Graph the standard additions data points, accounting for matrix interferences. Touch , then select and touch to view the relationship between View: Fit Ideal Line the sample spikes and the “Ideal Line” of 100% recovery. See Section 3.2.2 Standard Additions on page 32 for more information.
Page 485
Nitrogen, Ammonia Required Reagents Quantity Required Description per test Unit Cat. No. Low Range Test ’N Tube™ Nitrogen-Ammonia AmVer™ Reagent Set..... 25 tests ....26045-45 Required Apparatus Adapter, 16-mm Cell ................1 ....... each....59457-00 Funnel, micro, poly................... 1 ....... each....25843-35 ® Pipet, TenSette , 1.0–10.0 mL..............
Page 487
15 minutes and remain constant for another 15 minutes. • Underrange appears on the display when the instrument is zeroed or when the determined sample concentration is below the operating range listed for this method. UniCell Vials Hach Programs Hach Programs Touch Add 0.2 mL of sample...
Page 488
Nitrogen, Ammonium Zero HRS MIN SEC HRS MIN SEC Touch the timer icon. Install the 16-mm cell Touch When the timer Zero adapter. beeps, place the sample Touch The display will show: vial into the cell adapter. Note: See Section 2.6 Sample A 15-minute reaction 0.0 mg/L NH Cell Adapters in the Instrument...
Page 489
Nitrogen, Ammonium Accuracy Check Standard Additions Method (Sample Spike) 1. After reading test results, leave the sample cell (unspiked sample) in the instrument. 2. Touch . Touch . A summary of the standard Options Standard Additions additions procedure will appear. 3.
Page 491
15 minutes and remains constant for an additional 15 minutes. • Underrange appears on the display when the instrument is zeroed or when the determined sample concentration is below the operating range listed for this method. UniCell Vials Hach Programs Hach Programs Touch Add 5.0 mL of sample...
Page 492
Nitrogen, Ammonium Zero HRS MIN SEC HRS MIN SEC Touch the timer icon. Wipe the zero Install the 16-mm cell Touch Zero (white cap) and sample adapter. Touch The display will show: vials. Note: See Section 2.6 Sample A 15-minute reaction 0.00 mg/L NH Cell Adapters in the Instrument period will begin.
Page 493
Nitrogen, Ammonium Sample, Collection, Storage, and Preservation Analyze samples within 3 hours after collection for best results. Collect samples in clean plastic or glass bottles. To preserve samples for longer periods, add 1 mL of concentrated sulfuric acid per liter and store at 4 °C. Warm the sample to room temperature before testing.
Page 495
DR/2400 Nitrogen, Total Persulfate Digestion Method Method 10072 HR (10 to 150 mg/L N) Test ‘N Tube™ Vials Scope and Application: For water and wastewater. Tips and Techniques • Digestion is required for determining total nitrogen. The digestion procedure is included below. •...
Page 496
Nitrogen, Total Hach Programs Place the vials in the Using finger cots, Touch Remove the caps reactor. Heat for exactly immediately remove the from the digested vials Hach Programs 30 minutes. hot vials from the reactor. and add the contents of...
Page 497
Nitrogen, Total Zero Read Install the 16-mm Touch Wipe the reagent vial Touch Zero Read. adapter. and place it into the The display will show: Results will appear in adapter. mg/L N. Note: See Section 2.6 in the 0 mg/L N Instrument Manual for installation details.
Page 498
Accuracy Check This method generally yields 95–100% recovery on organic nitrogen standards. For proof of accuracy Hach offers a set of three Primary Standards for Kjeldahl Nitrogen (Cat. No. 22778-00). 1. Prepare one or more of the following three solutions. Each preparation is for an equivalent 120-mg/L N standard.
Page 499
Ammonia-PTSA Glycine-PTSA Nicotinic-PTSA Hach analysts have found Ammonia-PTSA to be the most difficult to digest. Other compounds may yield different percent recoveries. Standard Additions Method (Sample Spike) 1. After reading test results, leave the sample cell (unspiked sample) in the instrument.
Page 501
DR/2400 Nitrogen, Total Persulfate Digestion Method Method 10071 LR (0.5 to 25.0 mg/L N) Test ‘N Tube™ Vials Scope and Application: For water and wastewater Tips and Techniques • Digestion is required for determining total nitrogen. The digestion procedure is included below. •...
Page 502
Nitrogen, Total Hach Programs Place the vials in the Using finger cots, Touch Remove the caps reactor. Heat for exactly immediately remove the from the digested vials Hach Programs 30 minutes. hot vials from the reactor. and add the contents of...
Page 503
Nitrogen, Total Touch the timer icon. After the timer beeps, Cap the vials and Touch the timer icon. remove the caps from invert ten times to mix. Touch Touch two TN Reagent C vials Use slow, deliberate A two-minute reaction A five-minute reaction and add 2 mL of inversions for complete...
Page 504
Level and Effect Bromide > 60 mg/L; positive interference Chloride > 1000 mg/L; positive interference Hach chemists tested this chemistry on standard nitrogen solutions prepared from the following compounds and obtained 95% recovery: • Ammonium chloride • Urea • Ammonium sulfate •...
Page 505
Accuracy Check This method generally yields 95–100% recovery on organic nitrogen standards. For proof of accuracy Hach offers a set of three Primary Standards for Kjeldahl Nitrogen (Cat. No.22778-00). Use the deionized water included in the kit or water that is free of all organic and nitrogen-containing species.
Page 506
Nitrogen, Total Standard Additions Method (Sample Spike) 1. After reading test results, leave the sample cell (unspiked sample) in the instrument. Verify the chemical form. 2. Touch . Touch . A summary of the standard Options Standard Additions additions procedure will appear. 3.
Page 507
Nitrogen, Total Method Performance Precision Standard: 10 mg/L NH –N Program 95% Confidence Limits of Distribution 9.0–11.0 mg/L N See Section 3.4.3 Precision on page 44 for more information, or if the standard concentration did not fall within the specified range. Sensitivity ∆Abs ∆Concentration...
Page 509
• Use the standard solution or standard addition method to verify results. See Accuracy Check on page 3. • See Adjusting the Standard Curve on page 40 in the procedure manual for information on adjusting the calibration curve. UniCell Vials Hach Programs Hach Programs Touch Pipet 0.5 mL of...
Page 510
Nitrogen, Total Heat the reaction tube After the heating When the reaction Invert the tube in the reactor block at period, remove the tube tube has cooled to room several times until the 100 °C for 60 minutes. from the reactor block temperature, add a solid material in the cap and place it in a cooling...
Page 511
Nitrogen, Total Read Wipe the prepared Touch Read. sample and place it into Results will appear in the cell holder. mg/L N. Interferences The ions listed in the table have been tested up to the given concentrations. Cumulative effects and the influence of other ions have not been evaluated. Ions may interfere when present in conditions exceeding those listed below: Interfering Substance No interference up to:...
Page 512
Nitrogen, Total 4. Prepare three sample spikes by filling three mixing cylinders with 50 mL of sample. Use a pipet to add 0.2, 0.4, and 0.6 mL of 1000-mg/L NO –N Standard, respectively, to each sample and mix thoroughly. 5. Analyze each sample spike as described in the procedure above, starting with the 0.2 mL sample spike.
Page 513
Nitrogen, Total Summary of Method Bound nitrogen, both inorganically and organically bound, is oxidized to nitrate by digestion with peroxodisulphate. The nitrate ions react with 2,6-dimethylphenol in a solution of sulphuric and phosphoric acids to form a nitrophenol. Results are expressed as mg/L N or mg/L TN (Total Bound Nitrogen) with the same numeric value.
Page 515
>11 to prevent release of hydrogen cyanide gas. See Section 3 on page 27 for further information on proper disposal of these materials. • A green color will develop if inorganic nitrogen is present. Test ‘N Tube Method 10021 Hach Programs Hach Programs Touch Pipet 1 mL of Total Pipet 1 mL of sample...
Page 516
Nitrogen, Total Inorganic Pour the contents of Cap the vials. Shake Place the vials in a Touch the timer icon. one Total Inorganic gently for 30 seconds to centrifuge. Touch Nitrogen Reductant mix the reagents. Allow (If you do not have a A three-minute timer will ampule into the vial the vials to sit for at least...
Page 517
Nitrogen, Total Inorganic Zero Touch the timer icon. Install the 16-mm Touch Wipe the prepared Zero adapter. sample and place it into Touch The display will show: the cell holder. Note: See Section 2.6 in the A 20-minute reaction 0.0 mg/L N Instrument Manual for Touch Read.
Page 518
Nitrogen, Total Inorganic Sample Collection, Preservation, 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 (Cat. No. 323-32) for each 0.3 mg/L Cl in a one-liter sample.
Page 519
Nitrogen, Total Inorganic Method Performance The total inorganic nitrogen test is designed to provide an estimate of the total nitrite, nitrate, and ammonia nitrogen load present in a water or wastewater sample. This test is most applicable to the monitoring of samples taken from an industrial process stream or a wastewater treatment stream where it is important to track the inorganic nitrogen load as it passes through the treatment process.
Page 521
For water, wastewater, and sludge; digestion is required. * Adapted from Hach, et. al., Journal of Association of Official Analytical Chemists, 70(5) 783-787 (1987); Hach, et. al., Journal of Agricultural and Food Chemistry, 33(6) 1117-1123 (1985); Standard Methods for the Examination of Water and Wastewater Tips and Techniques •...
Page 522
Nitrogen, Total Kjeldahl If the aliquot is less Add 1.0 N KOH to Fill both cylinders to Add three drops of than 1 mL, proceed to each cylinder, one drop at the 20-mL mark with Mineral Stabilizer to each step 6. a time, mixing after each deionized water.
Page 523
Nitrogen, Total Kjeldahl Zero 10 mL 10 mL 10 mL 10 mL When the timer Wipe the blank and Touch Wipe the prepared Zero beeps, pour the contents place it into the cell sample and place it into The display will show: of each cylinder into holder.
Page 525
Nitrogen, Total Kjeldahl Method Performance Precision Standard: 120 mg/L NH –N Program 95% Confidence Limits of Distribution 107–133 mg/L NH –N See Section 3.4.3 Precision on page 44 for more information, or if the standard concentration did not fall within the specified range. Sensitivity ∆Abs ∆Concentration...
Page 527
DR/2400 Organic Carbon, Total Direct Method* Method 10128 HR (100 to 700 mg/L C) Scope and Application: For wastewater and industrial waters * U.S. Patent 6,368,870 Tips and Techniques • Place a safety shield in front of the COD reactor to prevent injury if splattering occurs. •...
Page 528
Do not touch the vial. Swirl to mix. ampules sides after wiping. Pick them up by the top. Hach Programs Lower one unopened Cap the vial Carefully remove the Touch ampule into each Acid assemblies tightly and...
Page 529
Organic Carbon, Total Zero Read Install the 16-mm cell Touch Wipe the reagent vial Touch Zero Read. adapter. assembly and place it into The display will show: Results will appear in the cell adapter. Note: See Section 2.6 Sample mg/L C. 0 mg/L C Cell Adapters in the Instrument Note: The display will show...
Page 530
Organic Carbon, Total (continued) Substance Maximum Level Tested 3– Phosphate 3390 mg/L PO Silica 100 mg/L SiO 2– Sulfate 5000 mg/L SO 2– Sulfide 20 mg/L S 2– Sulfite 50 mg/L SO Zinc 5 mg/L If the sample contains greater than 1000 mg/L CaCO alkalinity, lower the sample pH to less than 7 before testing by adding Sulfuric Acid Solution (Cat.
Page 531
Organic Carbon, Total Method Performance Precision Program mg/L C 95% Confidence Limits of Distribution ±14 mg/L C ±13 mg/L C ±15 mg/L C ±23 mg/L C ±34 mg/L C See Section 3.4.3 Precision on page 44 for more information, or if the standard concentration did not fall within the specified range.
Page 533
DR/2400 Organic Carbon, Total Direct Method* Method 10173 MR (15 to 150 mg/L C) Scope and Application: For wastewater and industrial waters * U.S. Patent 6,368,870 Tips and Techniques • Place a safety shield in front of the COD reactor to prevent injury if splattering occurs. •...
Page 534
Do not touch the vial. Swirl to mix. ampules sides after wiping. Pick them up by the top. Hach Programs Lower one unopened Cap the vial Carefully remove the Touch ampule into each Acid assemblies tightly and...
Page 535
Organic Carbon, Total Zero Read Install the 16-mm cell Touch Wipe the reagent vial Touch Zero Read. adapter. assembly and place it into The display will show: Results will appear in the cell adapter. Note: See Section 2.6 Sample mg/L C. 0 mg/L C Cell Adapters in the Instrument Note: The display will show...
Page 536
Organic Carbon, Total (continued) Substance Maximum Level Tested 3– Phosphate 3390 mg/L PO Silica 100 mg/L SiO 2– Sulfate 5000 mg/L SO 2– Sulfide 20 mg/L S 2– Sulfite 50 mg/L SO Zinc 5 mg/L If the sample contains greater than 1000 mg/L CaCO alkalinity, lower the sample pH to less than 7 before testing by adding Sulfuric Acid Solution (Cat.
Page 537
Organic Carbon, Total Method Performance Precision Program mg/L C 95% Confidence Limits of Distribution ±6 mg/L C ±3 mg/L C ±2 mg/L C ±5 mg/L C ±6 mg/L C See Section 3.4.3 Precision on page 44 for more information, or if the standard concentration did not fall within the specified range.
Page 539
DR/2400 Organic Carbon, Total Direct Method* Method 10129 LR (0.3 to 20.0 mg/L C) Scope and Application: For water, drinking water, and wastewater * U.S. Patent 6,368,870 Tips and Techniques • Place a safety shield in front of the COD reactor to prevent injury if splattering occurs. •...
Page 540
Do not touch the vial. Swirl to mix. ampules sides after wiping. Pick them up by the top. Hach Programs Lower one unopened Cap the vial Carefully remove the Touch ampule into each Acid assemblies tightly and...
Page 541
Organic Carbon, Total Zero Wipe the reagent Install the 16-mm cell Touch Wipe the sample vial Zero blank with a damp towel, adapter. assembly with a damp The display will show: followed by a dry one, to towel, followed by a dry Note: See Section 2.6 Sample 0.0 mg/L C remove fingerprints or...
Page 542
Organic Carbon, Total (continued) Substance Maximum Level Tested Chloride 500 mg/L Chlorine 10 mg/L Cl Chlorine Dioxide 6 mg/L ClO Copper 10 mg/L Cyanide 10 mg/L CN Iodide 50 mg/L Iron (II) 10 mg/L Iron (III) 10 mg/L Magnesium 2000 mg/L as CaCO Manganese (VII) 1 mg/L Monochloramine...
Page 543
Organic Carbon, Total 5. Continue the test starting at step 8 on page 2 of this procedure. 6. The mg/L C concentration should increase by 5.0 mg/L for each 0.1 mL increment. See Section 3.2.2 Standard Additions on page 32 for more information. Standard Solutions Method 1.
Page 545
DR/2400 Oxygen Demand, Chemical Reactor Digestion Method* Method 8000 (3 to 150, 20 to 1500, and 200 to 15,000 mg/L COD) Scope and Application: For water, wastewater, and seawater; digestion is required; 3–150 mg/L and 20– 1500 mg/L COD ranges are USEPA approved for wastewater analyses**; 200–15,000 mg/L COD range is not USEPA approved.
Page 546
Oxygen Demand, Chemical Hold one vial at a Hold a second vial at Cap the vials tightly. Hold the vials by the 45-degree angle. Use a a 45-degree angle. Use a Rinse them with cap over a sink. Invert clean volumetric pipet to clean volumetric pipet to deionized water and gently several times to...
Page 547
Oxygen Demand, Chemical Colorimetric Determination Method 8000 Hach Programs Zero Touch Clean the outside of Install the 16-mm Touch Zero the vials with a damp adapter. The display will show: Hach Programs towel followed by a dry Note: See Section 2.6 in the...
Page 548
Oxygen Demand, Chemical Blanks for Colorimetric Determination The blank may be used repeatedly for measurements using the same lot of vials. Store it in the dark. Monitor decomposition by measuring the absorbance at the appropriate wavelength (420 or 620 nm). Zero the instrument in the absorbance mode, using a vial containing 5 mL of deionized water and measure the absorbance of the blank.
Page 549
Oxygen Demand, Chemical Accuracy Check Standard Solution Method 1. Check the accuracy of the 3 to 150 mg/L range with a 100 mg/L standard. Prepare by dissolving 85 mg of dried (120 °C, overnight) potassium acid phthalate (KHP) in 1 liter of deionized water. Use 2 mL as the sample volume.
Page 550
Oxygen Demand, Chemical Method Performance Precision Standard: 80 mg/L COD (Low Range), 800 mg/L COD (High Range), and 10,000mg/L COD (High Range Plus) Program Range (mg/L) 95% Confidence Limits of Distribution 3–150 77.6–82.4 mg/L COD 20–1500 778–822 mg/L COD 200–15000 9778–10,222 mg/L COD See Section 3.4.3 Precision on page 44 for more information, or if the standard concentration did not fall within the specified range.
Page 551
Oxygen Demand, Chemical Required Reagents Quantity Required Description Per Test Unit Cat. No. Select the appropriate COD Digestion Reagent Vial: Low Range, 0 to 150 mg/L COD ............. 1 to 2 vials ..25/pkg....21258-25 High Range, 0 to 1,500 mg/L COD ..........1 to 2 vials ..25/pkg....21259-25 High Range Plus, 0 to 15,000 mg/L COD ........
Page 553
DR/2400 Oxygen Demand, Chemical Manganese III Reactor Digestion Method Method 10067 (with optional chloride removal)* (30 to 1000 mg/L COD Mn) Scope and Application: For water and wastewater * U.S. Patent 5,556,787 Tips and Techniques for Preparing the Acidified Sample ®...
Page 554
Oxygen Demand, Chemical Below Using an automatic Cap the cells tightly Proceed to Tips and dispenser (Cat. No. and invert several times. Techniques for Using the ® 25631-37) or TenSette Vacuum Pretreatment The solution will become Pipet, add 1.0 mL of Device on page 3.
Page 555
Oxygen Demand, Chemical Tips and Techniques for Using the Vacuum Pretreatment Device • If the sample does not flow through the Chloride Removal Cartridge (CRC), increase the vacuum until flow starts, then reduce the vacuum down to 20 inches of water. Proceed as usual. •...
Page 556
Oxygen Demand, Chemical Below Pipet 0.60 mL of Close the vacuum Open the VPD Proceed to Tips and acidified sample (see regulator valve regulator valve to release Techniques for Sample Preparing the Acidified completely to achieve full the vacuum. Turn the Preparation and Sample on page 1) into the vacuum.
Page 557
If the solution develops a several minutes. colorless upper layer and a purple lower layer, invert the vial several times to mix and proceed to the next step. 1.2" Hach Programs Zero 0.4" Touch Install the 16-mm Touch Make sure the filter Zero adapter.
Page 558
Accuracy Check Standard Solution Method 1. Purchase an 800-mg/L COD Standard Solution directly from Hach or prepare an 800-mg/L COD standard solution by adding 0.6808 g of dried (103 °C, overnight) potassium acid phthalate (KHP) to 1 liter of deionized water.
Page 559
Oxygen Demand, Chemical 3. Touch . Touch to accept the displayed concentration. If an alternate Adjust concentration is used, touch the number in the box to enter the actual concentration, then touch . Touch Adjust See Section 3.2.4 Adjusting the Standard Curve on page 40 for more information. Method Performance Note: Data is for Manganese III COD without the chloride removal procedure.
Page 561
• Place a safety shield in front of the COD reactor to prevent injury if splattering occurs. • Spilled reagent will affect test accuracy and is hazardous. Do not run tests with spilled vials. Without Chloride Removal Method 10067 Hach Programs Touch Turn on the COD Homogenize 100 mL Pipet 0.5 mL of...
Page 563
Scope and Application: For water and wastewater Tips and Techniques • Analyze samples on-site. Do not store for later analysis. AccuVac Ampul Method 8166 Hach Programs Hach Programs Touch Fill a round sample Fill a blue ampule cap Fill a High Range cell (the blank) with at with sample.
Page 564
Oxygen, Dissolved Zero Read HRS MIN SEC HRS MIN SEC Place the blank in the Place the ampule into Wait approximately Touch Read. cell holder. the cell holder. 30 seconds for the air Results will appear in bubbles to disperse from Touch mg/L O Zero...
Page 565
Oxygen, Dissolved Accuracy Check The results of this procedure may be compared with the results of a titrimetric procedure (request Lit. Code 8042) or sens ™6 Dissolved Oxygen Meter (Cat. No. 51850-01). Method Performance Precision Standard: 7.9 mg/L O Program 95% Confidence Limits of Distribution 7.5–8.3 mg/L O See Section 3.4.3 Precision on page 44 for more information, or if the standard...
Page 567
Tips and Techniques • The ampules will contain a small piece of wire to maintain reagent quality. The solution will be yellow. AccuVac Ampul Method 8316 Zero Hach Programs 10 mL Touch Fill a round sample Place the blank into...
Page 569
For aquaculture Tips and Techniques • Analyze samples on-site. Do not store for later analysis. AccuVac Ampul Method 8333 Hach Programs Touch Fill a round sample Fill a blue ampule cap Fill a High Range cell with at least 10 mL with sample.
Page 570
Oxygen, Dissolved Zero Read 10 mL Place the blank into Touch Place the AccuVac Touch Zero Read. the cell holder. Ampul into the cell The display will show: Results will appear in holder. mg/L O 0.0 mg/L O Interferences Interfering Substance Interference Levels and Treatments Greater than 10 mg/L Greater than 10 mg/L...
Page 571
Oxygen, Dissolved Accuracy Check The results of this procedure may be compared with the results of a titrimetric procedure (request Lit. Code 8042) or sens ™6 Dissolved Oxygen Meter (Cat. No. 51850-01). Method Performance Precision Standard: 36.0 mg/L O Program 95% Confidence Limits of Distribution 33.3–38.7 mg/L O See Section 3.4.3 Precision on page 44 for more information, or if the standard...
Page 573
• To determine ferrous iron concentration, repeat the procedure, but do not add DEHA Reagent 2 (step 5). Correct for the ferrous iron concentration by touching Options and Reagent Blank. Touch On. The reading attributed to the ferrous iron concentration will appear. Touch OK. Powder Pillows Method 8140 Hach Programs 25 mL 25 mL 25 mL 25 mL...
Page 574
Oxygen Scavengers 25 mL 20 mL Zero 25 mL 25 mL 10 mL 20 mL 20 mL 10 mL 10 mL Add 0.5 mL of DEHA Touch the timer icon. When the timer Touch Zero Reagent 2 Solution to beeps, wipe the blank Touch each sample cell.
Page 575
Oxygen Scavengers Interferences Interfering Substance Interference Levels and Treatments Borate (as Na Greater than 500 mg/L Cobalt Greater than 0.025 mg/L Copper Greater than 8.0 mg/L Ferrous Iron All levels Hardness (as CaCO Greater than 1000 mg/L Light Light may interfere. Keep sample cells in the dark during color development. Lignosulfonates Greater than 0.05 mg/L Manganese...
Page 577
• Use tap water or deionized water for the blank (ozone-free water). • The sequence of measuring the blank and the sample is reversed in this procedure. AccuVac Ampul Method 8311 Hach Programs Touch Gently collect at least Collect at least 40 mL...
Page 578
Ozone Zero Quickly invert both Wipe the ampules Place the sample into Touch Zero ampules several times to with a cloth to remove the cell holder. The display will show: mix. fingerprints or other 0.00 mg/L O marks. Some of the blue color will be bleached if ozone is present.
Page 579
Ozone Method Performance Precision Standard: 0.15 mg/L for program number 454 0.45 mg/L for program number 455 1.00 mg/L for program number 456 Program 95% Confidence Limits of Distribution 0.14–0.16 mg/L O 0.43–0.47 mg/L O 0.97–1.03 mg/L O See Section 3.4.3 Precision on page 44 for more information, or if the standard concentration did not fall within the specified range.
Page 581
• The Soil Extractant contains methyl alcohol which is poisonous and flammable. Before using this and other reagents, read the Material Safety Data Sheet (MSDS) for proper use of protective equipment and other safety information. • Hach Company recommends wearing protective nitrile gloves for this procedure. PCB (Polychlorinated Biphenyls) Page 1 of 10 PCB_None_Other_IMM_Eng_Ody.fm...
Page 582
PCB (Polychlorinated Biphenyls) Soil Extraction Procedure Weigh out 5 g of soil Carefully pour the Use the 5-gram scoop Use the graduated in the plastic weighing soil into an extraction to add one scoop of cylinder to transfer 10 mL boat.
Page 583
PCB (Polychlorinated Biphenyls) Immunoassay Procedure for Soil Extracts λ Touch Label an Antibody Place the cuvettes Pipet 0.5 mL of Cuvette for each snugly into the rack. Diluent Solution into Single Wavelength calibrator and each each cuvette. λ then touch the button.
Page 584
PCB (Polychlorinated Biphenyls) HRS MIN SEC HRS MIN SEC After 5 minutes, mix At the end of the Wash each cuvette the contents of the rack a 10-minute period, discard forcefully and thoroughly second time for a period the contents of all the four times with deionized of 30 seconds using the cuvettes into an...
Page 585
PCB (Polychlorinated Biphenyls) Color Development Note: Timing is critical; follow instructions carefully HRS MIN SEC HRS MIN SEC HRS MIN SEC HRS MIN SEC HRS MIN SEC HRS MIN SEC With the cuvettes still Touch the timer icon. After 2.5 minutes, At the end of the held snugly in the rack, Enter 5 minutes.
Page 586
PCB (Polychlorinated Biphenyls) Measuring the Color Zero Label and fill a Install the 1-cm Touch Place the first Zero Zeroing Cuvette with square cell adapter. calibrator into the cell The display will show: deionized water. Wipe holder. Note: See Section 2.6 Sample 0.000 Abs the outside of all the Cell Adapters in the Instrument...
Page 587
PCB (Polychlorinated Biphenyls) Figure 1 Wiretrol Pipet Wet the orange Push the tip to the Submerge the To discharge the ® Teflon tip of the Wiretrol other end of the capillary capillary tube below the pipet, place the tip of the plunger in the sample tube until it barely surface of the liquid to be...
Page 588
PCB (Polychlorinated Biphenyls) Figure 2 The 1-cm MicroCuvette Rack Loading the Rack — The cuvette rack is designed so that it may be inverted with the cuvettes in place. Identify each cuvette with a sample or calibrator number and place all the cuvettes in the rack before beginning the procedure. Fit the cuvettes snugly into the rack, but do not force them or they may be difficult to remove and their contents may spill.
Page 589
PCB (Polychlorinated Biphenyls) Interpretation Interpretation for a soil sample: Sample #1 — Sample reading is less than the readings for both calibrators. Therefore the sample concentration of PCB is greater than both 1 ppm and 5 ppm as Aroclor 1248. Sample #2 —...
Page 590
Soil Sample Container ....................20/pkg....25929-20 Weighing Boat, 8.9-cm square ..................20/pkg....21790-20 Spatula, disposable ...................... 2/pkg....25693-20 * Immunoassay components are manufactured for Hach Company by Beacon Analytical Systems, Inc. FOR TECHNICAL ASSISTANCE, PRICE INFORMATION AND ORDERING: HACH COMPANY In the U.S.A. –...
Page 591
>11 to prevent release of hydrogen cyanide gas. See Waste Management and Safety on page 55 for further information on proper disposal of these materials. Method 8047 Hach Programs Touch Measure 300 mL of...
Page 592
Phenols Pour the measured Add 5 mL of Add the contents of Add the contents of sample into another Hardness Buffer to each one Phenol Reagent one Phenol 2 Reagent 500-mL separatory funnel separatory funnel. Powder Pillow to each Powder Pillow to each (this is the prepared Stopper and shake to separatory funnel.
Page 593
Phenols 25 mL 25 mL 20 mL 20 mL Zero 25 mL 25 mL 20 mL 20 mL 10 mL 10 mL 10 mL 10 mL Drain the chloroform Wipe the blank and Touch Wipe the prepared Zero layers into separate place it into the cell sample and place it into The display will show:...
Page 594
Phenols Accuracy Check Standard Solution Method For greater accuracy, analyze standard solutions when new lots of reagent are first used. 1. Weigh out 1.00 g of Phenol, ACS. Transfer to a 1000-mL volumetric flask. Dilute to the mark with freshly boiled and cooled deionized water. This is a 1000-mg/L stock solution.
Page 595
This procedure is in the Hach Distillation Apparatus Manual in step-by-step illustrated format. 1. Set up the Hach Distillation Apparatus by assembling the general purpose apparatus as shown in the Distillation Apparatus Manual. Use the 500-mL Erlenmeyer flask to collect the distillate. It may be necessary to use a laboratory jack to elevate the flask.
Page 597
• The digestion in step 7 is normally completed in less than 10 minutes. However, contaminated samples or a weak lamp can cause incomplete phosphate conversion. Check conversion efficiency by running a longer digestion and seeing if the readings increase. Powder Pillows Method 8007 Hach Programs 10 mL Touch Choose the...
Page 598
Phosphonates Add the contents of Insert the ultraviolet Turn on the UV lamp. When the timer one Potassium Persulfate (UV) lamp into the Touch the timer icon. beeps, turn off the UV for Phosphonate Powder sample bottle. lamp and remove it from Touch Pillow to the bottle the sample.
Page 599
Phosphonates Zero 10 mL Table 1 Touch Wipe the prepared Multiply the value in Zero sample and place it into step 14 by the appropriate The display will show: the cell holder. multiplier in Table 1 to 3– 0.00 mg/L PO obtain the actual Touch Read.
Page 601
Standard Solution A 1-mg/L Phosphate Standard Solution (available from Hach) can be used to check accuracy. Use 10 mL of this standard in place of the prepared sample in step 9. Use deionized water for the blank. A multiplier value from Table 1 on page 3 is not needed.
Page 603
Federal RCRA. Please see Waste Management and Safety on page 55 for more information on proper disposal of these materials. Test ‘N Tube Method 8180 Hach Programs Turn on the COD Touch Use a TenSette Pipet Place the vial in the Reactor.
Page 604
Phosphorus, Acid Hydrolyzable Touch the timer icon. After the timer beeps, Using a TenSette Clean the outside of carefully remove the vial Pipet, add 2 mL of 1.00 N the vial with a towel to Touch from the reactor. Place it sodium hydroxide to the remove fingerprints or A 30-minute heating...
Page 605
Phosphorus, Acid Hydrolyzable Interferences Interfering Substance Interference Levels and Treatments Aluminum Greater than 200 mg/L Arsenate All levels Chromium Greater than 100 mg/L Copper Greater than 10 mg/L Iron Greater than 100 mg/L Nickel Greater than 300 mg/L Silica Greater than 50 mg/L Silicate Greater than 10 mg/L Greater than 9 mg/L.
Page 606
Phosphorus, Acid Hydrolyzable 5. Prepare three sample spikes. Fill three Mixing Cylinders (Cat. No. 1896-40) with 25 mL of sample. Use the TenSette Pipet to add 0.1 mL, 0.2 mL, and 0.3 mL of standard, respectively, to each sample and mix thoroughly. 6.
Page 607
Phosphorus, Acid Hydrolyzable Required Reagents Quantity Required Description Per Test Unit Cat. No Total and Acid Hydrolyzable Phosphorus Reagent Set..........50 tests ....27427-45 Includes: PhosVer 3 Phosphate Reagent Powder Pillows ......1 pillow... 50/pkg....21060-46 Potassium Persulfate Powder Pillows ..........1 ....... 50/pkg....20847-66 Sodium Hydroxide, 1.54 N ..................
Page 609
DR/2400 Phosphorus, Acid Hydrolyzable Digestion Acid Digestion Method* Method 8180 Scope and Application: For water, wastewater, and seawater; USEPA Accepted for wastewater analyses * Adapted from Standard Methods for the Examination of Water and Wastewater 4500-P B & E Tips and Techniques •...
Page 610
Phosphorus, Acid Hydrolyzable Digestion HRS MIN SEC HRS MIN SEC Use a 1-mL calibrated Pour the sample into Proceed with a dropper to add 2.0 mL of a 25-mL graduated reactive phosphorus test 5.0 N Sodium Hydroxide cylinder. Adjust the of the expected acid Solution to the flask.
Page 611
Phosphorus, Acid Hydrolyzable Digestion Summary of Method Phosphates present in condensed inorganic forms (meta-, pyro- or other polyphosphates) must be converted to reactive orthophosphate before analysis. Pretreatment of the sample with acid and heat hydrolyzes the condensed inorganic forms to orthophosphate. This procedure must be followed by one of the reactive phosphorus (orthophosphate) analysis methods for determining the phosphorus content of the sample.
Page 613
Subtract the reagent blank value from the final results. • Install the Pour-Thru Cell into the adapter so that the long pathlength (1-in./25-mm) is parallel to the front of the instrument. DR/2400 Pour-Thru Cell Method 10055 Hach Programs Touch Install the Pour-Thru Rinse two clean...
Page 614
Phosphorus, Reactive Fill this rinsed Pour the contents of Measure a second Add 1.0 mL of cylinder to the 25-mL the 25-mL cylinder into 25-mL portion of sample Molybdate reagent to mark with sample. one of the flasks. into the graduated each flask using a cylinder and pour the Repipet Jr.
Page 615
Phosphorus, Reactive Interferences Interfering Substance Interference Levels and Treatments Aluminum 200 mg/L Arsenate Interferes Chromium 100 mg/L Copper 10 mg/L Hydrogen sulfide Interferes Iron 100 mg/L Nickel 300 mg/L Silica 50 mg/L Silicate 10 mg/L Samples with large amounts of turbidity may give inconsistent results because the acid present Turbidity in the reagents may dissolve some of the suspended particles and variable desorption of orthophosphate from the particles may occur.
Page 616
Phosphorus, Reactive Sampling and Storage Collect samples in clean plastic or glass bottles that have been cleaned with 1:1 Hydrochloric Acid Solution (Cat. No. 884-49) and rinsed with deionized water. Do not use detergents that contain phosphate for cleaning labware. Analyze samples immediately for best results.
Page 617
Phosphorus, Reactive Method Performance Precision 3– Standard: 1000 µg/L PO Program 95% Confidence Limits of Distribution 3– 976–1024 µg/L PO See Section 3.4.3 Precision on page 44 for more information, or if the standard concentration did not fall within the specified range. Sensitivity ∆Abs ∆Concentration...
Page 619
• Substitute the contents of one Amino Acid Reagent Powder Pillow (Cat. No. 804-99) for 1 mL of amino acid reagent solution in step 4, if desired. Method 8178 Hach Programs Touch Fill a 25-mL mixing Add 1 mL of...
Page 620
Phosphorus, Reactive (Orthophosphate) 25 mL 20 mL Zero 25 mL 20 mL 10 mL 10 mL Touch the timer icon. Pour 25 mL of sample When the timer Touch Zero into a round sample cell beeps, place the blank Touch The display will show: (this is the blank).
Page 621
Phosphorus, Reactive (Orthophosphate) Interferences Interfering Substance Interference Levels and Treatments Calcium (Ca Greater than 10,000 mg/L as CaCO – Chloride Greater than 150,000 mg/L Cl Add 1 mL of 10 N Sulfuric Acid Standard Solution (Cat. No. 931-53) to another 25-mL sample. Colored samples Use this instead of untreated sample as the blank to zero the instrument.
Page 622
Phosphorus, Reactive (Orthophosphate) 3. Touch to accept the default values for standard concentration, sample volume, and spike volumes. Touch to change these values. After values Edit are accepted, the unspiked sample reading will appear in the top row. See Section 3.2.2 for more information. 3–...
Page 623
Phosphorus, Reactive (Orthophosphate) Summary of Method In a highly acidic solution, ammonium molybdate reacts with orthophosphate to form molybdophosphoric acid. This complex is then reduced by the amino acid reagent to yield an intensely colored molybdenum blue compound. Test results are measured at 530 nm.
Page 625
• For best results, sample temperature should be 20–25 °C (68–77 °F). • After adding reagent, a yellow color will form if phosphate is present. The blank will be slightly yellow because of the reagent. Reagent Solution Method 8114 Hach Programs 25 mL 25 mL 25 mL...
Page 626
0.0 mg/L PO Touch Read. period will begin. Results will appear in 3– mg/L PO AccuVac Ampul Method 8114 Hach Programs Touch Collect 40 mL of Fill a Touch the timer icon. sample in one 50-mL Molybdovanadate Touch Hach Programs beaker.
Page 627
Phosphorus, Reactive (Orthophosphate) Zero Read When the timer Touch Place the prepared Touch Zero Read beeps, place the blank sample into the cell The display will show: Results will appear in into the cell holder. holder. 3– mg/L PO 3– 0.0 mg/L PO Interferences Table 1 Interfering Substances and Suggested Treatments...
Page 628
Phosphorus, Reactive (Orthophosphate) The following do not interfere in concentrations up to 1000 mg/L: Table 2 Non-Interfering Substances Pyrophosphate Tetraborate selenate Benzoate Citrate Lactate Formate Oxalate Tartrate Salicylate – – 2– 2– – – 2– – – – 4– Sample Collection, Storage and Preservation Collect samples in clean plastic or glass bottles that have been cleaned with 1:1 Hydrochloric Acid Solution (Cat.
Page 629
Phosphorus, Reactive (Orthophosphate) , then select and touch to view the relationship between View: Fit Ideal Line the sample spikes and the “Ideal Line” of 100% recovery. See Section 3.2.2 Standard Additions on page 32 for more information. Standard Solution Method 1.
Page 631
• Final samples will contain molybdenum. Also, final samples will have a pH less than 2 and are considered corrosive (D002) by the Federal RCRA. Consult the Material Data Safety Data Sheet for information specific to the reagents used. Test ‘N Tube Method 8114 Hach Programs ® Touch Use a TenSette...
Page 632
Phosphorus, Reactive (Orthophosphate) Zero Read Install the 16-mm Touch Place the sample vial Touch Zero Read adapter. into the cell adapter. The display will show: Results will appear in 3– Note: See Section 2.6 in the mg/L PO 3– 0.0 mg/L PO Instrument Manual for installation details.
Page 633
Phosphorus, Reactive (Orthophosphate) Sampling and Storage Collect samples in plastic or glass bottles that have been cleaned with 1:1 Hydrochloric Acid Solution (Cat. No. 884-49) and rinsed with deionized water. Do not use commercial detergents containing phosphate for cleaning glassware used in this test. For best results, analyze the samples immediately after collection.
Page 635
Federal RCRA. Consult the Material Data Safety Data Sheet for information specific to the reagents used. • Install the Pour-Thru Cell into the adapter so that the long pathlength (1-in./25-mm) is parallel to the front of the instrument. DR/2400 Pour-Thru Cell Method 8114 Hach Programs Touch Install the Pour-Thru Rinse a clean plastic...
Page 636
Phosphorus, Reactive Rinse another clean Measure 25 mL of Add 1.0 mL of Touch the timer icon. plastic 125-mL sample in the graduated Molybdovanadate Touch Erlenmeyer flask and a cylinder. Pour the water Reagent to each flask A three-minute reaction 25-mL graduated into the flask (this is the using a Repipet Jr.
Page 637
Phosphorus, Reactive Interferences Interfering Substance Interference Levels and Treatments Arsenate Negative interference. Positive interference if sample is heated. Bismuth Negative interference. Fluoride Negative interference. Blue color is caused by ferrous iron but this does not affect results if the ferrous iron Iron, Ferrous concentration is less than 100 mg/L.
Page 638
Phosphorus, Reactive Sampling and Storage Collect samples in clean plastic or glass bottles that have been cleaned with 1:1 Hydrochloric Acid Solution (Cat. No. 884-49) and rinsed with deionized water. Do not use detergents that contain phosphate for cleaning labware. Analyze samples immediately for best results.
Page 639
Phosphorus, Reactive Standard Solution Method 1. Use a 10.0-mg/L Phosphate Standard in place of the sample. Results should be between 9.0 and 11.0 mg/L phosphate. 2. To adjust the calibration curve using the reading obtained with the 10-mg/L 3– Phosphate Standard Solution, touch on the current program Options menu.
Page 641
• Wipe the outside of sample cells before each insertion into the instrument cell holder. Use a damp towel followed by a dry one to remove fingerprints or other marks. Powder Pillows Method 8048 Hach Programs Touch Fill a sample cell with Add the contents of Touch the timer icon.
Page 642
Read Results will appear in 3– mg/L PO ® AccuVac Ampul Method 8048 Hach Programs 10 mL HRS MIN SEC HRS MIN SEC Touch Fill a sample cell with Fill a PhosVer 3 Place an ampule cap 10-mL of sample. (This is...
Page 643
Phosphorus, Reactive (Orthophosphate) Zero 10 mL Touch the timer icon. When the timer Touch Wipe the prepared Zero beeps, wipe the blank sample and place it into Touch The display will show: and place it into the cell the cell holder. 3–...
Page 644
Phosphorus, Reactive (Orthophosphate) Analyze samples immediately for best results. If prompt analysis is not possible, preserve samples by filtering immediately and storing at 4 °C (39 °F) for up to 48 hours. The sample should be at room temperature before analysis. Accuracy Check Standard Additions Method (Sample Spike) 1.
Page 645
Phosphorus, Reactive (Orthophosphate) Method Performance Precision 3– Standard: 1.00 mg/L PO Program 95% Confidence Limits of Distribution 3– 0.97–1.03 mg/L PO 3– 0.98–1.02 mg/L PO See Section 3.4.3 Precision on page 44 for more information, or if the standard concentration did not fall within the specified range. Sensitivity ∆Abs ∆Concentration...
Page 647
Subtract the reagent blank value from the final results or perform a reagent blank adjust Section 2.6.2 Reagent Blank on page 20 for more information. Test ‘N Tube Method 8048 Hach Programs ® Touch Use a TenSette...
Page 648
Phosphorus, Reactive (Orthophosphate) Zero Touch Using a funnel, add Cap the vial tightly Touch the timer icon Zero the contents of one and shake for 10–15 The display will show: Touch PhosVer 3 Phosphate seconds. The powder will 3– A two-minute reaction 0.00 mg/L PO Powder Pillow to the vial.
Page 649
Phosphorus, Reactive (Orthophosphate) (continued) Interfering Substance Interference Levels and Treatments (continued) Silicate Greater than 10 mg/L Greater than 6 mg/L. Remove sulfide interference as follows: 1. Measure 25 mL of sample into a 50-mL beaker. 2. Swirling constantly, add Bromine Water (Cat. No. 2211-20) Sulfide drop-wise until a permanent yellow color appears.
Page 650
Phosphorus, Reactive (Orthophosphate) 8. After completing the sequence, touch to view the best-fit line through Graph the standard additions data points, accounting for matrix interferences. Touch , then select and touch to view the relationship between View: Fit Ideal Line the sample spikes and the “Ideal Line”...
Page 651
Phosphorus, Reactive (Orthophosphate) Required Reagents Quantity Required Description Per Test Unit Cat. No. Reactive Phosphorus Test ’N Tube™ Reagent Set (50 tests)..............27425-45 Includes: ™ PhosVer 3 Phosphate Reagent Powder Pillows......1 ....... 50/pkg....21060-46 ........* Reactive Phosphorus Test ‘N Tube Dilution Vials......1 ....... 50/pkg Required Apparatus Adapter, 16-mm Cell ................
Page 653
• Underrange appears on the display when the instrument is zeroed or when the determined sample concentration is below the operating range listed for this method. UniCell Vials Hach Programs Touch Pipet 1.0 mL of Pipet 0.4 mL...
Page 654
Phosphorus, Reactive (Orthophosphate) HRS MIN SEC HRS MIN SEC Invert the sample vial Touch the timer icon Wipe the outside of Install the 16-mm cell repeatedly until the solid the zero (white cap) and adapter. Touch reagent in the cap sample vials with a damp Note: See Section 2.6 Sample A 10-minute reaction...
Page 655
Phosphorus, Reactive (Orthophosphate) (continued) Interfering Substance No interference up to: 50 mg/L 40 mg/L 25 mg/L 20 mg/L , Cr 10 mg/L 1 mg/L Sample Collection, Storage, and Preservation Analyze samples within 3 hours after collection for best results. Store in a cool dry place in plastic or glass bottles that have been acid cleaned with 1:1 Hydrochloric Acid Solution and rinsed with deionized water.
Page 657
• Underrange appears on the display when the instrument is zeroed or when the determined sample concentration is below the operating range listed for this method. UniCell Vials Hach Programs Touch Pipet 0.4 mL of Pipet 0.5 mL...
Page 658
Phosphorus, Reactive (Orthophosphate) HRS MIN SEC HRS MIN SEC Invert the sample vial Touch the timer icon Wipe the outside of Install the 16-mm cell repeatedly until the solid the zero (white cap) and adapter. Touch reagent in the cap is sample vials with a damp Note: See Section 2.6 Sample A 10-minute reaction...
Page 659
Phosphorus, Reactive (Orthophosphate) Sample Collection, Storage, and Preservation Analyze samples within 3 hours after collection for best results. Store in a cool dry place 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 phosphate for cleaning glassware used in this test.
Page 661
DR/2400 Phosphorus, Total, Digestion Acid Persulfate Digestion Method* Method 8190 Scope and Application: For water, wastewater, and seawater; USEPA Accepted for wastewater analyses * Adapted from Standard Methods for the Examination of Water and Wastewater 4500-P B & E Tips and Techniques •...
Page 662
Phosphorus, Total, Digestion HRS MIN SEC HRS MIN SEC Cool the sample to Use a 1-mL calibrated Pour the sample into Proceed with a room temperature. dropper to add 2.0 mL of a 25-mL graduated reactive phosphorus test 5.0 N Sodium Hydroxide cylinder.
Page 663
Phosphorus, Total, Digestion Summary of Method Phosphates present in organic and condensed inorganic forms (meta-, pyro-, or other polyphosphates) must be converted to reactive orthophosphate before analysis. Pretreatment of the sample with acid and heat provides the conditions for hydrolysis of the condensed inorganic forms. Organic phosphates are converted to orthophosphate by heating with acid and persulfate.
Page 665
• 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. Test ‘N Tube Method 8190 Hach Programs ® Turn on the COD Touch Use a TenSette...
Page 666
Phosphorus, Total Cap tightly and shake Place the vial into the Touch the timer icon. When the timer to dissolve. COD Reactor. beeps, carefully remove Touch the hot vial from the A 30-minute heating reactor. Place it in a test period will begin.
Page 667
Phosphorus, Total Use a funnel to add Cap tightly and shake Touch the timer icon. After the timer beeps, the contents of one to mix for 10–15 seconds. wipe the outside of the Touch PhosVer 3 Powder Pillow vial with a damp cloth The powder will not A two-minute reaction to the vial.
Page 668
Phosphorus, Total Interferences Interfering Substance Interference Levels and Treatments Aluminum Greater than 200 mg/L Arsenate Interferes at any level Chromium Greater than 100 mg/L Copper Greater than 10 mg/L Iron Greater than 100 mg/L Nickel Greater than 300 mg/L Highly buffered samples or extreme sample pH may exceed the buffering capacity of the pH, excess buffering reagents and require sample pretreatment.
Page 669
Phosphorus, Total 6. Prepare three sample spikes. Fill three Mixing Cylinders (Cat. No. 1896-40) with 25 mL of sample. Use the TenSette Pipet to add 0.1 mL, 0.2 mL, and 0.3 mL of standard, respectively, to each sample and mix thoroughly. 7.
Page 671
• The final samples will contain molybdenum. In addition, the final samples will have a pH less than 2 and are considered corrosive (D002) by the Federal RCRA. Consult the Material Data Safety Data Sheet for information specific to the reagents used. Test ‘N Tube Method 10127 Hach Programs ® Turn on the COD Touch...
Page 672
Phosphorus, Total Use a funnel to add Place the vials in the Touch the timer icon. After the timer beeps, the contents of one COD Reactor. carefully remove the hot Touch Potassium Persulfate vials from the reactor. A 30-minute heating Powder Pillow for Place them in a test tube period will begin.
Page 673
Phosphorus, Total Zero Read Install the 16-mm Touch Place the prepared Touch Zero Read adapter. sample into the cell The display will show: Results will appear in adapter. 3– Note: See Section 2.6 in the mg/L PO 3– 0.0 mg/L PO Instrument Manual for installation details.
Page 674
Phosphorus, Total Sampling and Storage Collect samples in plastic or glass bottles that have been acid washed with 1:1 Hydrochloric Acid Solution (Cat. No. 884-49) and rinsed with deionized water. Do not use commercial detergents containing phosphate for cleaning the glassware used in this test.
Page 675
Phosphorus, Total 3. Touch . Touch to accept the displayed concentration (the value Adjust depends on the selected chemical form). If an alternate concentration is used, touch the number in the box to enter the actual concentration, then touch Touch Adjust For more information, see Section 3.2.4 Adjusting the Standard Curve on page 40.
Page 677
• Underrange appears on the display when the instrument is zeroed or when the determined sample concentration is below the operating range listed for this method. UniCell Vials Hach Programs Touch Pipet 1.0 mL of Screw a blue...
Page 678
Phosphorus, Total Place the vial into the After the 60-minute Pipet 0.4 mL of Screw a light green Reactor Block. Heat at heating period, carefully Reagent B UniCap C (HCT 121 C) 100 °C for 60 minutes. remove the hot vial from (HCT 121/122 B) into the onto the sample vial.
Page 679
Phosphorus, Total Zero Read Touch Place the prepared Touch Zero Read sample vial into the cell The display will show: Results will appear in adapter. 3– mg/L PO 3– 0.0 mg/L PO Underrange Interferences The ions listed in the following table have been individually tested up to the given concentrations.
Page 680
Phosphorus, Total For wastewater samples — If prompt analysis is impossible, preserve samples by adjusting the pH to 2 or less with Sulfuric Acid, 5.25 N (Cat. No. 2449-00) and storing the sample at 4 °C for up to 28 days. The pH can be checked using pH Paper (Cat.
Page 681
Phosphorus, Total Method Performance Precision 3– Standard: 7.5 mg/L PO Program 95% Confidence Limits of Distribution 3– 7.2–7.8 mg/L PO See Section 3.4.3 Precision on page 44 for more information, or if the standard concentration did not fall within the specified range. Sensitivity ∆Abs ∆Concentration...
Page 683
• Underrange appears on the display when the instrument is zeroed or when the determined sample concentration is below the operating range listed for this method. UniCell Vials Hach Programs Touch Pipet 0.4 mL of Screw an orange...
Page 684
Phosphorus, Total Place the vial into the After the 60-minute Pipet 0.5 mL of Screw a grey Reactor Block. Heat at heating period, carefully Reagent B (HCT 121/ UniCap C (HCT 122 C) 100 °C for 60 minutes. remove the hot vial from 122 B) into the cooled onto the sample vial.
Page 685
Phosphorus, Total Interferences The ions listed in the following table have been individually tested up to the given concentrations. Cumulative effects and the influence of other ions have not been evaluated. Interfering Substance No interference up to: 2– 5000 mg/L –...
Page 686
Phosphorus, Total 6. Prepare three sample spikes. Fill three mixing cylinders with 25 mL of sample. Use a pipet to add 0.1 mL, 0.2 mL, and 0.3 mL of standard, respectively, to each cylinder. Mix well. 7. Analyze each sample spike as described in the procedure above, starting with the 0.1 mL sample spike.
Page 687
Phosphorus, Total Required Reagents Description Unit Cat. No. 3– Phosphate - PO , UniCell™ HCT 122................23/pkg....HCT 122 Required Apparatus Adapter, 16-mm Cell ......................each....59457-00 Optional Apparatus Cylinder, mixing, graduated 25-mL................. each....20886-40 Digital Reactor Block 100....................each....DRB 100 Pipettor, Jencons, 100–1000 µL..................each....27949-00 Rack, cooling, test tube ......................
Page 689
DR/2400 Potassium Tetraphenylborate Method Method 8049 (0.1 to 7.0 mg/L) Powder Pillows Scope and Application: For water, wastewater, and seawater Tips and Techniques • Program # 905 has a calibration curve for potassium; however, due to potential variation between lots of Potassium 3 Reagent, perform a new calibration for each lot of reagent to obtain best accuracy.
Page 690
Potassium 25 mL 20 mL 25 mL 25 mL 20 mL 20 mL 10 mL 10 mL 10 mL Touch the timer icon. Pour the solution When the timer Wipe the blank and from the cylinder into a beeps, fill the second place it into the cell Touch 25-mL sample cell (this is...
Page 691
Potassium Sample Collection, Preservation, and Storage Collect samples in acid-washed plastic bottles. Adjust the pH to 2 or less with Nitric Acid (about 2 mL per liter) (Cat. No. 2540-49). Preserved samples may be stored at least six months at room temperature. Before analysis, adjust the pH to 4–5 with 5.0 N Sodium Hydroxide (Cat.
Page 692
Potassium User Programming 1. Touch on the main menu. User Programs 2. If you have not performed a potassium calibration before, touch Program Options New Program 3. Assign a program number to the potassium user program. Touch 4. Select . Touch .
Page 693
Potassium Summary of Method Potassium in the sample reacts with sodium tetraphenylborate to form potassium tetraphenylborate, an insoluble white solid. The amount of turbidity produced is proportional to the potassium concentration. Test results are measured at 650. Required Reagents Quantity Required Description per test Unit...
Page 695
Method 8337 (0.2 to 5.0 mg/L as CTAB) Powder Pillows Scope and Application: For cooling tower water and pool/spa water Powder Pillows Method 8337 Hach Programs 25 mL 25 mL 25 mL 25 mL 25 mL 25 mL 20 mL...
Page 696
Quaternary Ammonium Compounds Interferences Interference studies were conducted by preparing a CTAB standard solution of approximately 3 mg/L as well as a solution of the potential interference. The constituent was said to interfere when the resulting concentration changed by 10%. Interfering Substance Interference Levels and Treatments Calcium (as CaCO...
Page 697
Quaternary Ammonium Compounds Sample Collection, Storage, and Preservation Collect samples in glass bottles that have been rinsed several times with sample before final sample filling. Do not use plastic containers as plastic adsorbs QACs. Acidify the sample to a pH of less than 2. Store at 4 ±2 °C. Accuracy Check Standard Additions Method (Sample Spike) 1.
Page 699
• If there are visible water bubbles on the bottom of the cell, decant the top portion into a clean, dry 10-mL cell prior to reading the sample. Method 8194 Hach Programs Touch Measure 100 mL of Add a 0.2-g spoonful Add a 0.05-g spoonful...
Page 700
Selenium If you have not Heat each flask on a Touch the timer icon. When the timer distilled the sample, add hot plate. Bring the beeps, remove both Touch 5.0 mL of Buffer Solution, contents to a gentle boil. flasks. Cool to room A five-minute reaction sulfate type, pH 2.0 to temperature using a...
Page 701
Selenium Touch the timer icon. Touch the timer icon. When the timer Insert a cotton plug beeps, drain the lower into the delivery tube of Touch Touch water layer from each each separatory funnel. A 30-second reaction A four-minute reaction funnel and discard.
Page 702
8. Cool the solution. While cooling, set up the distillation apparatus for the general purpose distillation as shown in the Hach Distillation Manual. 9. Pour the treated sample solution into the distillation flask. Add a stirring bar to the flask.
Page 703
Selenium 14. Fill a 250-mL beaker to the 75-mL mark with deionized water. Place it under the drip tube. Elevate the beaker with a laboratory jack so the tube extends below the level of the water. 15. Add 1.0 mL of 30% hydrogen peroxide solution to the flask. Turn the stir control to 5 and the heat control to 10.
Page 704
Selenium , then select and touch to view the relationship between View: Fit Ideal Line the sample spikes and the “Ideal Line” of 100% recovery. See Section 3.2.2 Standard Additions on page 32 for more information. Standard Solution Method Prepare a 0.5-mg/L Se standard solution as follows: 1.
Page 705
Selenium Required Reagents Quantity Required Description per test Unit Cat. No. Selenium Reagent Set (100 tests) ........................22442-00 Includes: (1) Buffer Solution, sulfate type, pH 2.0.......... 10 mL ....500 mL....452-49 (1) Diaminobenzidine, tetrahydrochloride........0.1 g....5 g......7062-22 (2) Potassium Hydroxide Standard Solution, 12 N....... 4 mL ....100 mL....230-32 ®...
Page 707
Scope and Application: For water and seawater Tips and Techniques • Sample temperature should be 15–25 °C (59–77 °F). Powder Pillows Method 8185 Hach Programs Touch Fill a round sample Add the contents of Add the contents of cell with 10-mL of...
Page 708
Silica Touch the timer icon. When the timer Touch the timer icon. Fill a second sample beeps, add the contents of cell with 10 mL of the Touch Touch one Citric Acid Powder original sample (the A ten-minute reaction A two-minute reaction Pillow to the sample cell.
Page 709
Silica Standard Methods for the Examination of Water and Wastewater under Silica-Digestion with Sodium Bicarbonate. A longer reaction time with the sample and the molybdate and acid reagents (before adding citric acid) may help instead of the bicarbonate treatment. Sample Collection, Storage, and Preservation Collect samples in clean plastic bottles.
Page 711
• The one-minute reaction time in step 6 is for samples at 20 °C; for samples at 10 °C, wait two minutes; for samples at 30 °C, wait 30 seconds. • If testing for very low levels of silica, use Method 8282. Powder Pillows Method 8186 Hach Programs 10 mL 10 mL Touch Fill two sample cells Add 14 drops of Touch the timer icon.
Page 712
Silica 10 mL When the timer Touch the timer icon. When the timer Touch the timer icon. beeps, add the contents of beeps, add the contents of Touch Touch one Citric Acid Reagent one Amino Acid F A one-minute reaction A two-minute reaction Powder Pillow to each Reagent Powder Pillow...
Page 713
Silica Interferences Interfering Substance Interference Levels and Treatments Color Eliminated by zeroing the instrument with the original sample. Iron Large amounts interfere. Does not interfere at levels less than 50 mg/L PO . At 60 mg/L PO , an interference of –2% occurs. Phosphate At 75 mg/L PO the interference is -11%.
Page 715
• Install the Pour-Thru Cell into the adapter so that the long pathlength (1-in./25-mm) is parallel to the front of the instrument. DR/2400 Pour-Thru Cell Method 8282 Options Reagent Blank: Hach Programs Adjust Return Touch Account for the To adjust the reagent...
Page 716
Silica Fill two clean 250-mL Fill a clean 50-mL Fill the rinsed Pour the contents of Erlenmeyer flasks to plastic graduated cylinder to the 50-mL the 50-mL cylinder back overflowing with sample. cylinder with sample mark with sample from into the original flask. from one of the flasks;...
Page 717
Silica Wait at least Flush the Pour-Thru 15 seconds, then pour the Cell with at least 50 mL of contents of the second deionized water flask into the Pour-Thru immediately after use. Cell. After the flow stops, touch Read Results will appear in µg/L SiO Interferences Interfering Substance...
Page 718
Silica Reagent Preparation Amino Acid F Reagent Solution is available in either 100-mL bottles or a package of 20 unit-dose ampules. The bottled reagent is stable for up to one year if the bottle is kept closed when not in use. The ampuled reagent is sealed under argon and is more stable with a shelf life greater than 1 year.
Page 719
Silica 3. Touch to accept the default values for standard concentration, sample volume, and spike volumes. Touch to change these values. After values Edit are accepted, the unspiked sample reading will appear in the top row. See Standard Additions in the instrument manual for more information. 4.
Page 721
• Install the Pour-Thru Cell into the adapter so that the long pathlength (1-in./25-mm) is parallel to the front of the instrument. DR/2400 Pour-Thru Cell Method 8282 Options Reagent Blank: Hach Programs Adjust Return Touch Account for the To adjust the reagent...
Page 722
Silica Fill two clean 250-mL Fill a clean 50-mL Fill the rinsed Pour the contents of Erlenmeyer flasks to plastic graduated cylinder to the 50-mL the 50-mL cylinder back overflowing with sample. cylinder with sample mark with sample from into the original flask. from one of the flasks;...
Page 723
Silica Zero Touch the timer icon. When the timer After the flow stops, Add 1.0 mL of Amino Touch beeps, pour the contents touch Acid F Reagent to the Zero of one flask into the remaining flask. Swirl to A one-minute reaction The display will show: Pour-Thru Cell.
Page 724
Silica Sample Collection, Storage, and Preservation Use only plastic containers with tight-fitting closures. Do not use glass containers; they will contaminate the sample with silica. Soak sampling containers with a solution made of one part Molybdate 3 Reagent (Cat. No. 1995-03) to 50 parts of high quality deionized water of low silica concentration.
Page 725
Silica Accuracy Check Standard Additions Method (Sample Spike) 1. After reading test results, leave the sample cell (unspiked sample) in the instrument. Verify the chemical form. 2. Touch . Touch . A summary of the standard Options Standard Additions additions procedure will appear. 3.
Page 726
In addition, the liquid reagents are directly used with Hach process analyzers for continuous silica measurement. Silica and phosphate in the sample react with molybdate ions under acidic conditions to form yellow silicomolybdic acid complexes and phosphomolybdic acid complexes.
Page 727
• Wipe the outside of sample cells before each insertion into the instrument cell holder. Use a damp towel followed by a dry one to remove fingerprints or other marks. Powder Pillows Method 8120 Hach Programs Hach Programs Touch Add the contents of...
Page 728
Silver 25 mL 25 mL 25 mL 20 mL 20 mL 20 mL 10 mL 10 mL 10 mL Fill a cell to the 25-mL Add the contents of Touch the timer icon. Fill a second cell to mark with the mixture. one Sodium Thiosulfate the 25-mL mark from the Touch...
Page 730
Silver Standard Solution Method Prepare a 0.5 mg/L silver standard solution as follows: 1. Pipet 0.50 mL of Silver Standard Solution, 1000 mg/L, into a 1000-mL volumetric flask using a Class A volumetric pipet. Dilute to the mark with deionized water. Prepare this solution daily. Perform the silver procedure as described above.
Page 731
Silver 3. Add 3 mL of concentrated sulfuric acid to the sample in the volumetric flask. Immediately place the head on the digestion flask. Never use less than 3 mL of acid. 4. Place the digestion flask on the heater. Turn the temperature dial to 440 °C (825 °F).
Page 733
4 contains barium chloride. The final solution will contain barium chloride (D005) at a concentration regulated as a hazardous waste by the Federal RCRA. See Section 4 for more information on proper disposal of these materials. Powder Pillows Method 8051 Hach Programs Touch Fill a clean sample Add the contents of Touch the timer icon.
Page 734
10 mL 10 mL Clean the sample cells with soap and a brush. AccuVac Ampul Method 8051 Hach Programs Touch Fill a clean sample Fill a SulfaVer 4 Quickly invert the cell with 10 mL of sample Sulfate AccuVac Ampul...
Page 735
Sulfate Zero 10 mL Wipe off any liquid or Touch the timer icon. When the timer Touch Zero fingerprints from the beeps, place the blank Touch The display will show: blank and the ampule. into the cell holder. 2– A five-minute reaction 0 mg/L SO period will begin.
Page 736
Sulfate Accuracy Check Standard Additions Method (Sample Spike) 1. After reading test results, leave the sample cell (unspiked sample) in the instrument. 2. Touch . Touch . A summary of the standard Options Standard Additions additions procedure will appear. 3. Touch to accept the default values for standard concentration, sample volume, and spike volumes.
Page 737
Sulfate Calibration Standard Preparation To perform a sulfate calibration using the SulfaVer method, use Class A glassware to prepare calibration standards containing 10, 20, 30, 40, 50, 60 and 2– 70 mg/L SO as follows: 1. Into seven different 100-mL Class A volumetric flasks, pipet 1, 2, 3, 4, 5, 6, and 7 mL of the 1000-mg/L Sulfate Standard Solution.
Page 739
• Underrange appears on the display when the instrument is zeroed or when the determined sample concentration is below the operating range listed for this method. UniCell Vials Hach Programs Touch Add 5 mL of sample Add one spoonful Immediately cap the to a sample vial.
Page 740
Sulfate Zero Wipe the outside of Install the 16-mm cell Touch Place the sample in Zero the zero (white cap) and adapter. the cell adapter. The display will show: sample vials with a damp Note: See Section 2.6 Sample Touch Read 2–...
Page 741
Sulfate 3. Touch to accept the default values for standard concentration, sample volume, and spike volumes. Touch to change these values. After values Edit are accepted, the unspiked sample reading will appear in the top row. 4. Prepare three sample spikes. Fill three mixing cylinders with 25 mL of 2–...
Page 743
• Underrange appears on the display when the instrument is zeroed or when the determined sample concentration is below the operating range listed for this method. UniCell Vials Hach Programs Touch Add 2 mL of sample Add one spoonful of Immediately cap the to a sample vial.
Page 744
Sulfate Zero HRS MIN SEC HRS MIN SEC Touch the timer icon. Wipe the outside of Install the 16-mm cell Touch Zero the zero (white cap) and adapter. Touch The display will show: sample vials with a damp Note: See Section 2.6 Sample 2–...
Page 745
Sulfate Sample Collection, Storage, and Preservation Analyze samples within 3 hours after collection for best results. Samples may be stored up to 28 days at 4 °C (39 °F). Warm samples to room temperature before analysis. Accuracy Check Standard Additions Method (Sample Spike) 1.
Page 747
• Sulfide 2 reagent contains potassium dichromate. The final solution will contain hexavalent chromium (D007) at a concentration regulated as a hazardous waste by Federal RCRA. Please see Section 4 for further information on proper disposal of these materials. Method 8131 Hach Programs 25 mL 25 mL 25 mL...
Page 748
Sulfide 25 mL 20 mL Zero 25 mL 25 mL 20 mL 20 mL 10 mL 10 mL 10 mL Use the calibrated 1- Touch the timer icon. When the timer Touch Zero mL dropper to add beeps, wipe the blank Touch The display will show: 1.0 mL of Sulfide 2...
Page 749
Sulfide Interferences Interfering Substance Interference Levels and Treatments Strong reducing substances (sulfite, thiosulfate and Interfere by reducing the blue color or preventing its development hydrosulfite) High concentrations of sulfide may inhibit full color development and require sample dilution. Sulfide, high levels Some sulfide loss may occur when the sample is diluted.
Page 751
• Samples must be analyzed immediately. • Sample and Reagent temperature must be between 15–25 °C (59–77 °F). • Adjust the sample pH between 3–10. Colorimetric Method Hach Programs Touch Fill a clean sample Pipet 10 mL of Add 5 drops of Sulfite...
Page 752
Sulfite Zero 10 mL Add 2 drops of Touch the timer icon. Wipe the blank and Touch Zero Sulfite Reagent B place the it into the cell Touch The display will show: (HPT 430 B). holder. 2– A 3-minute reaction 0.00 mg/L SO Swirl to mix.
Page 753
Sulfite Accuracy Check Standard Additions Method (Sample Spike) 1. After reading test results, leave the sample cell (unspiked sample) in the instrument. 2. Touch . Touch . A summary of the standard Options Standard Additions additions procedure will appear. 3. Touch to accept the default values for standard concentration, sample volume, and spike volumes.
Page 755
Subtract the reagent blank value from the final results or perform a reagent blank adjust See the instrument manual for more information on Running a Reagent Blank. Method 8028 Hach Programs Touch Fill a clean 500-mL Add 10 mL of Sulfate...
Page 756
Surfactants, Anionic (Detergents) Add 30 mL of Place the separatory Touch the timer icon. After the timer beeps, benzene to the funnel. funnel in a support stand. remove the stopper and Touch Stopper the funnel and drain the bottom water A 30-minute reaction shake gently for one layer.
Page 757
Surfactants, Anionic (Detergents) Interferences Interfering Substance Interference Levels and Treatments High amounts of chloride, such as those levels found in brines Chloride and seawater, will cause low results. Perchlorate ions Interferes at all levels. Periodate ions Interferes at all levels. Sample Collection, Storage, and Preservation Collect samples in clean plastic or glass bottles.
Page 759
Scope and Application: For water and wastewater * Adapted from Sewage and Industrial Wastes, 31, 1159 (1959). Method 8006 HRS MIN SEC HRS MIN SEC Hach Programs 25 mL 20 mL 10 mL Touch Blend 500 mL of Pour the blended...
Page 761
• Filter turbid samples and report results as mg/L soluble tannic acid. • Results will be given in mg/L tannins (as tannic acid). ® • For best accuracy, use a pipet to add the TanniVer 3 solution. Method 8193 Hach Programs Hach Programs 25 mL 25 mL 25 mL 25 mL...
Page 762
Tannin and Lignin 25 mL 20 mL Zero 25 mL 25 mL 20 mL 20 mL 10 mL 10 mL 10 mL Pipet 5.0 mL of Touch the timer icon. When the timer Touch Zero Sodium Carbonate beeps, place the blank Touch The display will show: Solution into each cell.
Page 763
Tannin and Lignin Accuracy Check Standard Solution Method Prepare a 200-mg/L tannic acid standard solution as follows: 1. Dissolve 0.200 grams of tannic acid in deionized water and dilute to 1000 mL. Prepare this solution monthly. Further prepare a 6.0-mg/L tannic acid standard by diluting 15.00 mL of the stock solution to 500 mL with deionized water.
Page 765
DR/2400 Toxicity ToxTrak™ Method * ** Method 10017 (0 to 100% Inhibition) Scope and Application: For water and wastewater * U.S. Pat. No. 5,413,916 ** Liu, D., Bull. Environ. Contm. Toxicol. 26, 145-149 (1981) Tips and Techniques • Do not leave the cells in the instrument during incubation. All samples and control cells should be allowed to react under similar conditions of temperature and light.
Page 766
Toxicity Inoculum Development Using Aqua QC-Stiks Inoculate a Lauryl Incubate the Lauryl Inoculate a new Invert the new tube. Tryptose broth tube with Tryptose Broth Tube at Lauryl Tryptose Broth After incubation, this an E. coli Aqua QC-Stik™ 35 °C (95 °F) until the Tube by first inverting new vial may be used in according to the...
Page 767
Toxicity Repeat Zero Step 6 Touch Label a cell “control”. For each sample or Add 5.0 mL of Zero Open one ToxTrak dilution, repeat step 6. deionized water to the The display will show: Reagent Powder Pillow control cell. Label each cell. 0.000 ABS and add the contents to Use deionized water that...
Page 768
Toxicity Repeat Zero Step 12 HRS MIN SEC HRS MIN SEC Repeat step 12 for all Allow the solutions in After the absorbance Touch Zero samples and dilutions. Be the tubes to react until the of the control has The display will show: sure to record each absorbance of the control decreased to 0.60 ±0.10...
Page 769
Toxicity Interpreting Results The % Inhibition results obtained are only a relative measurement. They do not represent a true quantitative measurement of toxic concentration. The % Inhibition does not necessarily increase in direct proportion to the concentration of toxins. To determine the minimum inhibition concentration of a toxin, it is possible to make tenfold dilutions of the sample and determine the % Inhibition for the dilutions until the sample is diluted sufficiently so that no inhibition is observed.
Page 771
• The Soil Extractant contains methyl alcohol which is poisonous and flammable. Before using this and other reagents, read the Material Safety Data Sheet (MSDS) for proper use of protective equipment and other safety information. • Hach Company recommends wearing protective nitrile gloves for this procedure. TPH (Total Petroleum Hydrocarbons) Page 1 of 12 TPHSoil_None_Other_IMM_Eng_Ody.fm...
Page 772
TPH (Total Petroleum Hydrocarbons) Soil Extraction Procedure Weigh out 10 g of soil Carefully pour the Use the 5-gram scoop Use the graduated in the plastic weighing soil into an extraction to add one scoop of cylinder to transfer 10 mL boat.
Page 773
TPH (Total Petroleum Hydrocarbons) Immunoassay Procedure for Soil Extracts and Water Samples λ Touch Label an Antibody Place the cuvettes Pipet 0.5 mL of Cuvette for each into the rack snugly. Diluent Solution into Single Wavelength calibrator and each each Calibrator cuvette. λ...
Page 774
TPH (Total Petroleum Hydrocarbons) If testing soil: Pipet Have the necessary If testing soil: Use a Immediately pipet 0.5 mL of Diluent Solution apparatus at hand for the Wiretrol pipet to transfer 0.5 mL of TPH Enzyme into each sample cuvette. next four steps as they 50 µL of the filtered Conjugate into each...
Page 775
TPH (Total Petroleum Hydrocarbons) Wash each cuvette forcefully and thoroughly four times with deionized water. Empty the rinse water into the waste container. Note: Ensure most of the water is drained from the cuvettes by turning the cuvettes upside down and tapping them lightly on a paper towel.
Page 776
TPH (Total Petroleum Hydrocarbons) Measuring the Color Zero Label and fill a Install the 1-cm Touch Place the first Zero Zeroing Cuvette with square cell adapter. calibrator into the cell The display will show: deionized water. Wipe holder. Note: See Section 2.6 Sample 0.000 Abs the outside of all the Cell Adapters in the Instrument...
Page 777
TPH (Total Petroleum Hydrocarbons) ® Using the Wiretrol Pipet The Wiretrol Pipet can accurately measure small quantities of liquids. It consists ® of two parts: a Teflon -tipped plunger and a calibrated capillary tube. Use Figure 1 to determine the quantity measured at each line on the capillary tube. The plunger can be re-used;...
Page 778
TPH (Total Petroleum Hydrocarbons) Using the 1-cm MicroCuvette Rack This rack (see Figure 2) has been designed specifically to aid in achieving precise and accurate results when using the immunoassay technique to analyze several samples at the same time. Figure 2 The 1-cm MicroCuvette Rack Loading the Rack —...
Page 779
TPH (Total Petroleum Hydrocarbons) Sample #2: 0.400 Abs Sample #3: 0.550 Abs Interpretation Interpretation for a soil sample: Sample #1 — Sample reading is less than the readings for both calibrators. Therefore the sample concentration of TPH is greater than both 20 ppm and 50 ppm diesel fuel.
Page 780
TPH (Total Petroleum Hydrocarbons) Table 1 Various TPHs in Soil calibrator #1 calibrator #2 calibrator #3 calibrator #4 Compound Diesel Gasoline Kerosene Benzene Toluene Ethylbenzene m-Xylene o-Xylene p-Xylene BTEX Table 2 Various TPHs in Water calibrator #1 calibrator #2 calibrator #3 calibrator #4* Compound Diesel...
Page 781
Water 2, 5, 10, 20 ppm as diesel fuel Hach immunoassay tests use antigen/antibody reactions to test for specific organic compounds in water and soil. Antibodies specific for TPH are attached to the walls of plastic cuvettes. They selectively bind and remove TPH from complex sample matrices.
Page 782
Soil Sample Container ....................20/pkg....25929-20 Spatula, disposable ...................... 2/pkg....25693-20 Weighing Boat, 8.9-cm square ..................20/pkg....21790-20 * Immunoassay components are manufactured for Hach Company by Beacon Analytical Systems, Inc. FOR TECHNICAL ASSISTANCE, PRICE INFORMATION AND ORDERING: HACH COMPANY In the U.S.A. –...
Page 783
Volatile Acids Esterification Method* Method 8196 (27 to 2800 mg/L) Scope and Application: For digestor sludges * Adapted from The Analyst, 87, 949 (1962) Method 8196 Hach Programs 25 mL 25 mL 20 mL 20 mL 10 mL 10 mL Touch Pipet 0.5 mL of...
Page 784
Volatile Acids 25 mL 25 mL 25 mL 20 mL 20 mL 20 mL 25 mL 25 mL 25 mL 25 mL 25 mL 25 mL 10 mL 10 mL 10 mL 20 mL 20 mL 20 mL 20 mL 20 mL 20 mL 10 mL...
Page 785
Volatile Acids 25 mL 20 mL Read 10 mL Wipe the prepared Touch Read sample and place it into Results will appear in the cell holder. mg/L HOAC. Sample Collection, Preservation, and Storage Collect samples in clean plastic or glass bottles. Analyze as soon as possible after collection.
Page 786
Volatile Acids Standard Solution Method Prepare a 500 mg/L volatile acid standard solution as follows: 1. Pipet 4.00 mL of a 62,500-mg/L Volatile Acid Standard Solution into a 500-mL Class A volumetric flask. Dilute to volume with deionized water. Prepare this solution daily. Perform the esterification procedure as described above.
Page 787
Volatile Acids Required Reagents Quantity Required Description Per Test Unit Cat. No. Volatile Acids Reagent Set (90 tests) ......................22447-00 Includes: (1) Ethylene Glycol................3 mL ....1000 mL....2039-53 (2) Ferric Chloride-Sulfuric Acid Solution ........20 mL ....1000 mL....2042-53 (1) Hydroxylamine Hydrochloride Solution, 100-g/L ....1 mL ....100 mL....818-42 (1) Sodium Hydroxide Standard Solution, 4.5 N ......
Page 789
>11 to prevent release of hydrogen cyanide gas. See Section 4 for further information on proper disposal of these materials. Powder Pillows Method 8009 Hach Programs Touch Fill a 25-mL Add the contents of Invert several times...
Page 790
Zinc 10 mL Pour 10 mL of the Use a plastic dropper Touch the timer icon Touch the timer icon. solution into a sample to add 0.5 mL of Touch Touch cell (this is the blank). cyclohexanone to the A 30-second reaction A three-minute reaction remaining solution in the period will begin.
Page 791
Zinc Interferences Interfering Substance Interference Levels and Treatments Aluminum Greater than 6 mg/L Cadmium Greater than 0.5 mg/L Copper Greater than 5 mg/L Iron (ferric) Greater than 7 mg/L Manganese Greater than 5 mg/L Nickel Greater than 5 mg/L Organic Material Large amounts may interfere.
Page 792
Zinc 7. After completing the sequence, touch to view the best-fit line through Graph the standard additions data points, accounting for matrix interferences. Touch , then select and touch to view the relationship between View: Fit Ideal Line the sample spikes and the “Ideal Line” of 100% recovery. See Section 3.2.2 Standard Additions on page 32 for more information.
Page 793
Zinc Summary of Method Zinc and other metals in the sample are complexed with cyanide. Adding cyclohexanone causes a selective release of zinc. The zinc then reacts with 2-carboxy-2'-hydroxy-5'-sulfoformazyl benzene (zincon) indicator to form a blue-colored species. The blue color is masked by the brown color from the excess indicator.
Page 795
• Underrange appears on the display when the instrument is zeroed or when the determined sample concentration is below the operating range listed for this method. UniCell Vials Hach Programs Touch Pipet 4 mL of sample Pipet 0.4 mL of Immediately cap into a sample vial.
Page 796
Zinc Zero Invert the sample vial Touch the timer icon. Install the 16-mm cell Touch Zero repeatedly until the adapter. Touch The display will show: solids in the cap dissolve Note: See Section 2.6 Sample An 3-minute reaction 0.00 mg/L Free Zn completely.
Page 797
Zinc Sample Collection, Preservation, and Storage Collect samples in acid-cleaned glass or plastic containers. No acid addition is necessary if analyzing the samples immediately. To preserve samples, adjust the pH to 2 or less with concentrated nitric acid (about 2 mL per liter). Preserved samples may be stored up to six months at room temperature.