HACH 8000: Oxygen Demand, Chemical Using Reactor Digestion
Contents
1. CPRIIFICA Ty By Authority Of THE UNITED STATES OF AMERICA Legally Binding Document By the Authority Vested By Part 5 of the United States Code 552 a and Part 1 of the Code of Regulations 51 the attached document has been duly INCORPORATED BY REFERENCE and shall be considered legally binding upon all citizens and residents of the United States of America HEED THIS NOTICE Criminal penalties may apply for noncompliance Y Document Name HACH 8000 Oxygen Demand Chemical Using Reactor Digestion Method CFR Section s 40 CFR 136 3 a Standards Body Hach Chemical Company Official Incorporator THE EXECUTIVE DIRECTOR OFFICE OF THE FEDERAL REGISTER WASHINGTON D C Oxygen Demand Chemical DOC316 53 01099 USEPA Reactor Digestion Method Method 8000 0 7 to 40 03 mg L COD ULR 3 to 150 mg L COD LR 20 to 1500 mg L COD HR 200 to 15 000 mg L COD HR Plus Scope and Application For water wastewater digestion is required 1 Ranges 3 to 150 mg L COD and 20 to 1500 mg L COD are USEPA approved for wastewater analyses Standard Method 5220 D Federal Register April 21 1980 45 78 26811 26812 2 Jirka A M Carter M J Analytical Chemistry 1975 47 8 1397 3 The ULR range is not available on the DR 2700 or the DR 2400 Test preparation How to use instrument specific information The nstrument specific information table displays requirements that may vary between ins2. Description Quantity Unit Catalog number Blender 2 speed 120 VAC 1 each 2616100 OR Blender 2 speed 240 VAC 1 each 2616102 DRB200 Reactor 110 V 15 x 16 mm 1 each LTV082 53 40001 OR DRB200 Reactor 220 V 15 x 16 mm 1 each LTV082 52 40001 Pipet Filler safety bulb 1 each 1465100 Pipet Volumetric Class A 2 00 mL 1 each 1451536 Oxygen Demand Chemical Page 9 of 12 Oxygen Demand Chemical Recommended standards and apparatus Description Unit Catalog number Beaker 250 mL each 50046H COD Standard Solution 300 mg L 200 mL 1218629 COD Standard Solution 300 mg L 500mL 1218649 COD Standard Solution 800 mg L 200 mL 2672629 COD Standard Solution 1000 mg L 200 mL 2253929 Oxygen Demand Standard BOD COD TOC 10 mL ampules 16 pkg 2833510 Pipet TenSette 0 1 to 1 0 mL each 1970001 Pipet Tips for TenSette Pipet 1970001 50 pkg 2185696 Pipet Tips for TenSette Pipet 1970001 1000 pkg 2185628 Potassium Acid Phthalate ACS 500 g 31534 Stir Bar 28 6 x 7 9 mm each 2095352 Stirrer Electromagnetic 120 VAC with electrode stand each 4530001 Stirrer Electromagnetic 230 VAC with electrode stand each 4530002 Test Tube Rack 16 mm each 1864100 Wipes Disposable 70 pkg 2096900 Optional reagents and apparatus Description Unit Catalog number Balance analytical 80 g capacity 115 VAC each 2936701 Flask volumetric 1000 mL Class A each 1457453 Flask volumetric 100 mL Class A each 1457442 Mercuric Sulfate 28g 1915
3. 20 Pipet volumetric 3 mL Class A each 1451503 Pipet volumetric 10 mL Class A each 1451538 Sulfuric Acid conc 500 mL 97949 Wastewater Influent Standard for mixed parameters NH3 N NO3 N PO4 COD SO4 500mL 2833149 TOC Wastewater Effluent Standard for mixed parameters NH3 N NO3 N PO4 COD SO4 500mL 2833249 TOC Weighing Paper 76x76 mm 500 pkg 1473800 Finger cots 2 pkg 1464702 Gloves chemical resistant 9 9 2 1 pair 2410104 Safety goggles vented each 2550700 EZ COD Recycling Service with 5 gal2 bucket mail back each 2895405 EZ COD Recycling Service with 5 gal bucket pick up3 each 2895405P 1 Other sizes are available 2 20 and 55 gal are available 3 ez COD available to U S customers only Oxygen Demand Chemical Page 10 of 12 Oxygen Demand Chemical Oxygen Demand Chemical Page 11 of 12 HACH COMPANY FOR TECHNICAL ASSISTANCE PRICE INFORMATION AND ORDERING In the U S A Call toll free 800 227 4224 WORLD HEADQUARTERS Outside the U S A Contact the HACH office or distributor serving you Telephone 970 669 3050 FAX 970 669 2932 On the Worldwide Web www hach com E mail techhelp hach com Edition 6 Hach Company 2007 2010 All rights reserved Printed in the U S A
4. Oxygen Demand Chemical Page 8 of 12 Consumables and replacement items Required reagents Description Select the appropriate COD Digestion Reagent Vial Ultra Low Range 0 7 to 40 mg L COD Low Range 3 to 150 mg L COD High Range 20 to 1500 mg L COD High Range Plus 200 to 15 000 mg L COD Water deionized Alternate reagents Description Select the appropriate COD Digestion Reagent Vial COD2 Low Range 0 to 150 mg L COD COD2 High Range 0 to 1500 mg L COD COD2 High Range 0 to 1500 mg L COD COD2 High Range Plus 0 to 15 000 mg L COD COD Digestion Reagent Vials 3 to 150 mg L COD COD Digestion Reagent Vials 200 to 1500 mg L COD COD Digestion Reagent Vials ULR 0 7 40 0 mg L COD Digestion Reagent Vials HR plus 200 25 000 mg L Oxygen Demand Chemical Quantity Test Unit 1 2 vials 25 pkg 1 2 vials 25 pkg 1 2 vials 25 pkg 1 2 vials 25 pkg varies 4L Quantity Test Unit 1 2 vials 25 pkg 1 2 vials 25 pkg 1 2 vials 150 pkg 1 2 vials 25 pkg 1 2 vials 150 pkg 1 2 vials 150 pkg 1 2 vials 150 pkg 1 2 vials 150 pkg Catalog number 2415825 2125825 2125925 2415925 27256 Catalog number 2565025 2565125 2565115 2834325 2125815 2125915 2415815 2415915 1 These reagents are not approved for USEPA reporting purposes Request a copy of the COD2 Reagent Vial Information Brochure Lit No 1356 for more information about specific applications Required apparatus
5. e vial 6 Blank Preparation Hold a second vial at a 45 degree angle Use a clean volumetric pipet to add 2 00 mL of deionized water to the vial For the 200 15 000 mg L vials Use a TenSette Pipet to add 0 20 mL of deionized water to the vial 9 Heat the vials for two hours 10 Turn the reactor off Before removing the vials wait about 20 minutes for the vials to cool to 120 C or less i 7 Cap the vials tightly Rinse them with water and wipe with a clean paper towel 11 Invert each vial several times while still warm 8 Hold the vials by the cap over a sink Invert gently several times to mix The sample vials become very hot during mixing Insert the vials in the preheated DRB200 Reactor Close the protective lid 12 Place the vials into a rack and cool to room temperature Proceed to Colorimetric determination Oxygen Demand Chemical Page 3 of 12 Oxygen Demand Chemical Colorimetric determination Stored Programs 431 COD ULR Start 1 Select the test 2 Clean the outside of 3 Insert the blank into 4 ZERO the instrument Insert an adapter or light the vials with a damp towel the 16 mm cell holder The display will show shield if required see followed by a dry one 0 mg L COD Instrument specific or information 0 0 mg L COD Refer to the user manual for orientation oncforr Read oume OnE EIEEEI nE LIA 5 Insert the sample
6. equired for accuracy check 1000 mg L COD Standard Solution OR Potassium acid phthalate KHP dried overnight at 120 C Deionized water organic free Class A volumetric flasks Class A volumetric pipet 0 7 to 40 0 mg L range 1 Prepare a 30 mg L COD standard solution as follows a Pipet 3 00 mL of the 1000 mg L standard into a 100 mL volumetric flask b Dilute to volume with deionized water and mix well Use 2 mL of the 30 mg L COD solution in place of the sample Follow the Colorimetric determination test procedure The result should be 30 mg L Refer to the Standard adjust instructions in this procedure to adjust the curve with the reading obtained from the standard 3 to 150 mg L range 1 Prepare a 100 mg L COD standard solution as follows a Pipet 10 mL of the 1000 mg L standard into a 100 mL volumetric flask b Dilute to volume with deionized water and mix well Use 2 mL of the 100 mg L solution in place of the sample Follow the Colorimetric determination test procedure The result should be 100 mg L Refer to the Standard adjust instructions in this procedure to adjust the curve with the reading obtained from the standard 20 to 1500 mg L range Use 2 mL of 300 mg L 800 or 1000 mg L COD standards for accuracy check Oxygen Demand Chemical Page 6 of 12 Oxygen Demand Chemical 200 to 15 000 mg L range 1 Prepare a 10 000 mg L COD standard solution as follows a Dissolve 8 500 g of dried KHP in 1000 mL
7. gent vials varies DRB200 Reactor 1 Light Shield or adapter see nstrument specific information 1 Magnetic stirrer and stir bar 1 Opaque shipping container for storage of unused light sensitive reagent vials varies Pipet TenSette 0 1 to 1 0 mL with tips for 200 15 000 mg L range 1 Pipet volumetric 2 00 mL 2 Pipet Filler safety bulb 1 Test Tube Rack 2 See Consumables and replacement items for reorder information Reactor digestion procedure fee E 1 Homogenize 100 mL 2 For the 200 3 Turn on the DRB200 4 Remove the caps from of sample for 30 seconds 15 000 mg L range or to Reactor Preheat to two COD Digestion in a blender For samples improve accuracy and 150 C Reagent Vials Be sure to containing large amounts reproducibility of the other See the DRB200 User use vials for the of solids increase the ranges pour the Manual for selecting pre appropriate range homogenization time homogenized sample into programmed temperature a 250 mL beaker and applications gently stir with a magnetic stir plate If the sample does not contain suspended solids omit steps 1 and 2 Oxygen Demand Chemical Page 2 of 12 Reactor digestion procedure continued Oxygen Demand Chemical 4 A 5 Prepared Sample Hold one vial at a 45 degree angle Use a clean volumetric pipet to add 2 00 mL of sample to the vial For the 200 15 000 mg L vials Use a TenSette Pipet to add 0 20 mL of sample to th
8. of organic free deionized water 2 Use 0 2 mL of the 10 000 mg L COD solution in place of the sample Follow the Colorimetric determination test procedure The result should be 10 000 mg L after multiplying by 10 Refer to the Standard adjust instructions in this procedure to adjust the curve with the reading obtained from the standard Standard adjust 1 To adjust the calibration curve using the reading obtained with the standard solution navigate to Standard Adjust in the software OPTIONS gt MORE gt STANDARD ADJUST 2 Turn on the Standard Adjust feature and accept the displayed concentration If an alternate concentration is used enter the concentration and adjust the curve to that value Alternate reagents Mercury free COD2 Reagents can provide a mercury free testing option for non reporting purposes For process control applications COD2 Reagents will eliminate mercury waste and save on disposal costs These reagents are fully compatible with test procedures and calibration curves programmed into the spectrophotometer Determine chloride and ammonia for accurate results Important Note COD2 reagents are not approved for USEPA reporting purposes Because COD2 reagents do not contain mercury as a masking agent they exhibit a positive interference from chloride Request a copy of the COD2 Reagent Vial Information Brochure Lit No 1356 for more information about specific applications Oxygen Demand Chemical Page 7 of 12 O
9. tion to be too low for accurate determination add 0 50 g of mercuric sulfate HgSO to each COD vial before the sample is added The additional mercuric sulfate will raise the maximum chloride concentration allowable to the level given in Column 3 Column 3 Maximum chloride Table 2 Interfering substances concentration with Column 2 comm Suggested chloride Vial range Maximum chloride 99 l l concentration for concentration i diluted samples mercuric sulfate Ultra Low Range 1 2000 1000 N A 0 7 40 0 mg L Low Range 2000 1000 8000 3 150 mg L High Range 2000 1000 4000 20 1500 mg L High Range Plus 20 000 10 000 40 000 200 15 000 mg L 1 Ultra Low Range is not available on the DR 2700 Sample collection preservation and storage e Collect samples in glass bottles e Use plastic bottles only if they are known to be free of organic contamination e Test biologically active samples as soon as possible e __Homogenize samples containing solids to assure representative samples e Samples treated with sulfuric acid to a pH of less than 2 about 2 mL per liter and refrigerated at 4 C can be stored up to 28 days e Correct the test results for volume additions See Optional reagents and apparatus Oxygen Demand Chemical Page 5 of 12 Oxygen Demand Chemical Accuracy check Standard solution method Note Refer to the instrument user manual for specific software navigation instructions R
10. truments To use this table select an instrument then read across to find the corresponding information required to perform this test Table 1 Instrument specific information Instrument Light shield DR 3900 LZV849 DR 3800 DR 2800 LZV646 Before starting the test DR 3900 DR 3800 DR 2800 and DR 2700 Install the light shield in Cell Compartment 2 before performing this test Some of the chemicals and apparatus used in this procedure may be hazardous to the health and safety of the user if inappropriately handled or accidentally misused Please read all warnings and associated MSDS sheets Run one blank with each set of samples Run all tests the samples and the blank with the same lot of vials The lot number appears on the container label See Blanks for colorimetric determination Spilled reagent will affect test accuracy and is hazardous to skin and other materials Be prepared to wash spills with running water Wear appropriate eye protection and clothing for adequate user protection If contact occurs flush the affected area with running water Review and follow reagent MSDS safety instructions carefully Store unused light sensitive vials in a closed box If high chloride samples are being tested refer to the Alternate reagents section Oxygen Demand Chemical Page 1 of 12 Oxygen Demand Chemical Collect the following items Description Quantity Beaker 250 mL 1 Blender 1 COD Digestion Rea
11. vial 6 READ the results in 7 If using High Range into the 16 mm mg L COD Plus COD Digestion Reagent Vials multiply the result by 10 For most accurate results with samples near 1500 or 15 000 mg L COD repeat the analysis with a diluted sample Blanks for colorimetric determination The blank may be used repeatedly for measurements using the same lot of vials Store the blank in the dark 1 Monitor decomposition by measuring the absorbance at the appropriate wavelength Refer to the Range specific test wavelengths table 2 Zero the instrument in the absorbance mode Use a vial containing 5 mL of deionized water and measure the absorbance of the blank Record the value 3 Prepare a new blank when the absorbance has changed by about 0 01 absorbance units Oxygen Demand Chemical Page 4 of 12 Oxygen Demand Chemical Interferences Chloride is the primary interference when determining COD concentration Each COD vial contains mercuric sulfate that will eliminate chloride interference up to the level specified in Column 1 of the nterfering substances table Dilute samples with higher chloride concentrations Dilute the sample enough to reduce the chloride concentration to the level given in Column 2 Note For best results use the low range and ultra low range test for samples with high chloride concentrations approaching maximum concentration and low COD concentrations If sample dilution will cause the COD concentra
12. xygen Demand Chemical Method performance Precision Sensitivity Program Standard 95 Confidence Limits of Concentration change Distribution per 0 010 Abs change 430 77 83 mg L COD 3 mg L COD Range 80 mg L COD Low Range 3 150 mg L 431 28 8 31 2 mg L COD 0 5 mg L COD 30 mg L COD Ultra Low Ranger Range 0 5 40 0 mg L 435 785 815 mg L COD 23 mg L COD Range 800 mg L COD High Range 20 1500 mg L l 8000 mg L COD High Range 7850 8150 mg L COD 230 mg L COD 200 15 000 mg L PIB Summary of method The results in mg L COD are defined as the milligrams of O consumed per liter of sample under the conditions of this procedure The sample is heated for two hours with sulfuric acid and a strong oxidizing agent potassium dichromate Oxidizable organic compounds react reducing the dichromate ion Cr2O072 to green chromic ion Cr When the 0 7 40 0 or the 3 150 mg L colorimetric method is used the amount of Cr6 remaining is determined When the 20 1500 mg L or 200 15 000 mg L colorimetric method is used the amount of Cr3 produced is determined The COD reagent also contains silver and mercury ions Silver is a catalyst and mercury is used to complex chloride interferences Test results are measured at the wavelengths specified in the Range specific test wavelengths table Table 3 Range specific test wavelengths Range in mg L COD Wavelength 0 7 to 40 0 mg l 1 Not available on the DR 2700
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