HACH 8008: 1, 10--Phenanthroline Method Using FerroVer Iron
Contents
1. CERTMAICATE 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 WW Document Name HACH 8008 1 10 Phenanthroline Method Using FerroVer Iron Reagent for Water 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 Iron j Total DOC316 53 01053 USEPA1 FerroVer Method2 Method 8008 0 02 to 3 00 mg L Powder Pillows or AccuVac Ampuls Scope and Application For water wastewater and seawater digestion is required for determining total iron 1 USEPA approved for reporting wastewater analysis Federal Register June 27 1980 45 126 43459 2 Adapted from Standard Methods for the Examination of Water and Wastewater Test preparation How to use instrument specific information The nstrument specific information table displays requirements that may vary between instruments To use this table select an instrument then read across to find the corresponding information required to perform this test Table 1 Instrument specif2. as described in the FerroVer method for AccuVac Ampuls Accept each standard additions reading Each addition should reflect approximately 100 recovery Standard solution method Note Refer to the instrument user manual for specific software navigation instructions Required for accuracy check Iron Standard Solution 100 mg L 100 mL volumetric flask Class A volumetric pipet 2 mL Deionized water Pipet filler Prepare a 2 00 mg L Fe standard solution as follows a Pipet 2 00 mL of Iron Standard Solution 100 mg L into a 100 mL volumetric flask b Dilute to the mark with deionized water Mix well Prepare this solution daily Use the 2 00 mg L Fe standard solution in place of the sample Follow the FerroVer method for powder pillows test procedure To adjust the calibration curve using the reading obtained with the Standard Solution select Options gt More gt Standard Adjust from the instrument menu 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 Mixed parameter standards are also available to simulate various matrices Method performance Precision Sensitivity Program Standard 95 Confidence Limits of Concentration change Distribution per 0 010 Abs change 265 2 00 mg L Fe 1 99 2 01 mg L Fe 0 021 mg L Fe 267 2 00 mg L Fe 1 98 2 02 mg L Fe 0 023 mg L Fe lron Total P
3. 4 of 8 lron Voluette Ampule Standard 25 mg L Ampule breaker TenSette Pipet and Pipet Tips After reading test results leave the sample cell unspiked sample in the instrument Select Options gt More gt Standard Additions from the instrument menu Accept the default values for standard concentration sample volume and spike volumes After the values are accepted the unspiked sample reading will appear in the top row See the user manual for more information Open the standard solution ampule Prepare a 0 1 mL sample spike by adding 0 1 mL of standard to 10 mL of unspiked sample Start the instrument timer After the timer expires read the result Iron Total Prepare a 0 2 mL sample spike by adding 0 1 mL of standard to the 0 1 mL sample spike Start the instrument timer After the timer expires read the result Prepare a 0 3 mL sample spike by adding 0 1 mL of standard to the 0 2 mL sample spike Start the instrument timer After the timer expires read the result Select GRAPH to view the results Select IDEAL LINE or best fit to compare the standard addition results to the theoretical 100 recovery Standard additions method for AccuVac Ampuls sample spike 1 Fill three mixing cylinders each with 50 mL of sample and spike with 0 2 mL 0 4 mL and 0 6 mL of standard Stopper and invert to mix Transfer 40 mL from each of the three mixing cylinders to three 50 mL beakers Analyze each standard addition sample
4. age 5 of 8 Iron Total Summary of method FerroVer Iron Reagent converts all soluble iron and most insoluble forms of iron in the sample to soluble ferrous iron The ferrous iron reacts with the 1 10 phenanthroline indicator in the reagent to form an orange color in proportion to the iron concentration Test results are measured at 510 nm Consumables and replacement items Required reagents Description Quantity Test Unit Catalog number FerroVer Iron Reagent Powder Pillows for 10 mL sample 1 100 pkg 2105769 OR FerroVer Iron Reagent AccuVac Ampuls 1 25 pkg 2507025 Required apparatus Description Quantity Unit Catalog number Beaker 50 mL 1 each 50041H Sample cell 10 mL round 25 x 54 mm 1 each 2122800 Sample cell 10 mL round 25 x 60 mm 1 6 pkg 2427606 Sample cell 10 mL square matched pair 2 2 pkg 2495402 Stopper for 18 mm tube 1 6 pkg 173106 Recommended standards Description Unit Catalog number Iron Standard Solution 100 mg L 100 mL 1417542 Iron Standard Solution 10 mL Voluette Ampule 25 mg L as Fe 16 pkg 1425310 Metals Drinking Water Standard LR for Cu Fe Mn 500 mL 2833749 Metals Drinking Water Standard HR for Cu Fe Mn 500 mL 2833649 Water deionized 4L 27256 Pipet TenSette 0 1 1 0 mL each 1970001 Pipet Tips for TenSette Pipet 1970001 50 pkg 2185696 Pipet Tips for TenSette Pipet 1970001 1000 pkg 2185628 Flask volumetric Class A 100 mL each 1457442 Pi
5. eorder information FerroVer method for powder pillows Stored Programs 265 Iron FerroVer Start 1 Select the test Insert an adapter if required see nstrument specific information Refer to the user manual for orientation 10 mL 4 5 Blank preparation Fill a second sample cell with 10 mL of sample Iron Total Page 2 of 8 C 10 mL 4 2 Prepared sample Fill a clean sample cell with 10 mL of sample 6 When the timer expires insert the blank into the cell holder 3 Add the contents of one FerroVer Iron Reagent Powder Pillow to the sample cell Swirl to mix Accuracy is not affected by undissolved powder 7 ZERO the instrument The display will show 4 Start the instrument timer A three minute reaction period will begin An orange color will form if iron is present Allow samples that contain rust to react for at least 5 minutes 8 Insert the prepared sample into the cell holder READ the results in mg L Fe Iron Total FerroVer method for AccuVac Ampuls Stored Programs 267 Iron FerroVer AV Start Won mp on 2 Blank Preparation Fill a round sample cell with 10 mL of sample 1 Select the test Insert an adapter if required see nstrument specific information 3 Prepared Sample Collect at least 40 mL of Fill a FerroVer Iron AccuVac Ampul with sample from the beaker Keep the tip immersed wh
6. ic information Powder pillows AccuVac Ampuls Instrument Sample cell Cell orientation Sample cell Adapter DR 5000 2495402 Fill line faces user 2427606 DR 3900 2495402 Fill line faces user 2427606 LZV846 A DR 3800 DR 2800 DR 2700 2495402 Fill line faces right 2122800 LZV584 C Before starting the test Digestion is required for determining total iron for EPA reporting purposes Use the mild or vigorous digestion Refer to the Water Analysis Guide for more information For more accurate results determine a reagent blank value for each new lot of reagent Follow the procedure using deionized water in place of the sample Subtract the reagent blank value from the final results or perform a reagent blank adjust See the user manual for more information Adjust pH of stored samples before analysis For turbid samples treat the blank with one 0 1 g scoop of RoVer Rust Remover Swirl to mix Collect the following items Description Quantity Powder Pillow Test FerroVer Iron Reagent Powder Pillow 1 Sample Cells see nstrument specific information 2 Iron Total Page 1 of 8 Iron Total Collect the following items continued Description Quantity AccuVac Ampul test Beaker 50 mL Stopper of 18 mm tubes FerroVer Iron Reagent AccuVac Ampul Sample Cells see nstrument specific information See Consumables and replacement items for r
7. ile the Ampul fills completely Refer to the user manual for orientation os OK 03 00 5 Start the instrument timer Zero 7 ZERO the instrument The display will show 0 00 mg L Fe 6 Wipe the blank and insert it into the cell holder A three minute reaction period will begin An orange color will develop if iron is present Interferences Table 2 Interfering substances sample in a 50 mL beaker 4 Quickly invert the Ampul several times to mix Accuracy is not affected by undissolved powder 8 Wipe the Ampul and insert it into the cell holder READ the results in mg L Fe Interfering substance Interference level Calcium Ca2 No effect at less than 10 000 mg L as CaCO3 Chloride CI No effect at less than 185 000 mg L Copper Cu2 No effect Masking agent is contained in FerroVer Reagent High Iron Levels Inhibit color development Dilute sample and re test to verify results lromQxide sodium hydroxide then analyze Requires mild vigorous or Digesdahl digestion After digestion adjust sample to pH 3 5 with Magnesium No effect at 100 000 mg L as calcium carbonate Iron Total Page 3 of 8 Iron Total Table 2 Interfering substances continued Interfering substance Interference level Molybdate Molybdenum No effect at 50 mg L as Mo High Sulfide Levels S2 1 Treat in fume hood or well ventilated area Add 5 mL hydroch
8. loric acid ACS to 100 mL sample in a 250 mL Erlenmeyer flask Boil 20 minutes 2 Cool Adjust pH to 3 5 with Sodium Hydroxide Readjust volume to 100 mL with deionized water 3 Analyze using FerroVer method for powder pillows or FerroVer method for AccuVac Ampuls Turbidity 1 Add 0 1 g scoop of RoVer Rust Remover to the blank Swirl to mix Zero the instrument with this blank 3 If sample remains turbid add three 0 2 g scoops of RoVer to a 75 mL sample Let stand 5 minutes 4 Filter through a Glass Membrane Filter and Filter Holder 5 Use the filtered sample as the prepared sample and the blank Extreme Sample pH Adjust pH to 3 5 Highly Buffered Samples Adjust pH to 3 5 1 See Optional reagents and apparatus Sample collection preservation and storage Collect samples in acid cleaned glass or plastic containers No acid addition is necessary if analyzing the sample immediately To preserve samples adjust the pH to 2 or less with concentrated nitric acid about 2 mL per liter Preserved samples may be stored up to six months at room temperature Before analysis adjust the pH to between 3 and 5 with 5 0 N Sodium Hydroxide Standard Solution Correct the test result for volume additions If only dissolved iron is to be determined filter the sample before acid addition Accuracy check Standard additions method sample spike Required for accuracy check Iron Total Page
9. pet volumetric Class A 2 00 mL each 1451536 Pipet Filler safety bulb each 1465100 Optional reagents and apparatus Description Unit Catalog number Beaker 50 mL each 50041H Cylinder mixing 50 mL each 189641 Hydrochloric Acid concentrated 500 mL 13449 Nitric Acid concentrated 500 mL 15249 iron Total Page 6 of 8 Optional reagents and apparatus continued Iron Total Description Unit Catalog number Sodium Hydroxide Standard Solution 5 0 N 100 mL 245032 Glass Membrane Filter 47 mm 100 pkg 253000 Glass Membrane Filter Holder each 234000 RoVer Rust Remover 454 g 30001 Spoon measuring 0 1 g each 51100 Iron Total Page 7 of 8 Iron Total HACH COMPANY Bins FOR TECHNICAL ASSISTANCE PRICE INFORMATION AND ORDERING N In the U S A Call toll free 800 227 4224 WORLD HEADQUARTERS SG p Outside the U S A Contact the HACH office or distributor serving you Telephone 970 669 3050 ARREDO On the Worldwide Web www hach com E mail techhelp hach com FAX 970 669 2932 Edition 6 Hach Company 2007 2010 All rights reserved Printed in the U S A
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