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54

SAMPLE PRETREATMENT

, continued

EPA Vigorous Digestion with Hot Plate for Metals Analysis Only

A vigorous digestion can be followed to ensure all organo-metallic bonds
are broken.

1.

Acidify the entire sample with redistilled 1:1 Nitric Acid Solution to a
pH of less than two. Do not filter the sample before digestion.

2.

Transfer an appropriate sample volume (see

Table 8

) into a beaker

and add 3 mL of concentrated redistilled nitric acid.

3.

Place the beaker on a hot plate and evaporate to near dryness, making
certain the sample does not boil.

4.

Cool the beaker and add another 3 mL of the concentrated redistilled
nitric acid.

5.

Cover the beaker with a watch glass and return it to the hot plate.
Increase the temperature of the hot plate so that a gentle reflux occurs.
Add additional acid, if necessary, until the digestion is complete
(generally indicated when the digestate is light in color or does not
change color or appearance with continued refluxing).

6.

Again, evaporate to near dryness (do not bake) and cool the beaker. If
any residue or precipitate results from the evaporation, add redistilled
1:1 hydrochloric acid (5 mL per 100 mL of final volume). See

Table 8

.

7.

Warm the beaker. Add 5 mL of 5.0 N sodium hydroxide and
quantitatively transfer the sample with deionized water to a
volumetric flask. See

Table 8

below for the suggested final volume.

8.

Adjust the sample to pH 4 by drop-wise addition of 5.0 N Sodium
Hydroxide Standard Solution; mix thoroughly and check the pH after
each addition. Dilute to volume with deionized water. Multiply the
result by the correction factor in

Table 8

. A reagent blank also should

be carried through the digestion and measurement procedures.

Table 8 Vigorous Digestion Volumes

Expected Metal

Concentration

Suggested Sample

Vol. for Digestion

Suggested Volume

of 1:1 HCl

Suggested Final

Volume After

Digestion

Correction Factor

1 mg/L

50 mL

10 mL

200 mL

4

10 mg/L

5 mL

10 mL

200 mL

40

100 mg/L

1 mL

25 mL

500 mL

500

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Содержание DR/850

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

Страница 2: ...2...

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

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

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

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

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

Страница 8: ...8...

Страница 9: ...9 Sample Procedure Explained...

Страница 10: ...10 Sample Procedure Explained continued...

Страница 11: ...11 Sample Procedure Explained continued...

Страница 12: ...12 Sample Procedure Explained continued...

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

Страница 69: ...69 SECTION 4 PROCEDURES...

Страница 70: ...70...

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

Страница 92: ...92...

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

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

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

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

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

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

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

Страница 100: ...100...

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

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

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

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

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

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

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

Страница 108: ...108...

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

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

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

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

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

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

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

Страница 116: ...116...

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

Страница 139: ...139...

Страница 140: ...140...

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

Страница 168: ...168...

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

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

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

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

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

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

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

Страница 176: ...176...

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

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

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

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

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

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

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

Страница 184: ...184...

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

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

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

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

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

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

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

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

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

Страница 194: ...194...

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

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

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

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

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

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

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

Страница 202: ...202...

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

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

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

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

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

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

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

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

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

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

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

Страница 214: ...214...

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

Страница 234: ...234...

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

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

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

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

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

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

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

Страница 242: ...242...

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

Страница 264: ...264...

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

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

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

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

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

Страница 270: ...270...

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

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

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

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

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

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

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

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

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

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

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

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

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

Страница 284: ...284...

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

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

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

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

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

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

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

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

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

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

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

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

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

Страница 298: ...298...

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

Страница 314: ...314...

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

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

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

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

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

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

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

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

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

Страница 324: ...324...

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

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

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

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

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

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

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

Страница 332: ...332...

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

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

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

Страница 336: ...336...

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

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

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

Страница 340: ...340...

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

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

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

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

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

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

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

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

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

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

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

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

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

Страница 354: ...354...

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

Страница 370: ...370...

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

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

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

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

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

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

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

Страница 378: ...378...

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

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

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

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

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

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

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

Страница 386: ...386...

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

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

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

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

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

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

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

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

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

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

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

Страница 398: ...398...

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

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

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

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

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

Страница 404: ...404...

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

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

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

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

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

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

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

Страница 412: ...412...

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

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

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

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

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

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

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

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

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

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

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

Страница 424: ...424...

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

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

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

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

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

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

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

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

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

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

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

Страница 436: ...436...

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

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

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

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

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

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

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

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

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

Страница 446: ...446...

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

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

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

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

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

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

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

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

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

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

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

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