Manual - Hach Nickel Reagent Set
Contents
1. Nickel DOC316 53 01064 USEPA Heptoxime Method Method 8037 0 02 to 1 8 mg L Ni Powder Pillows Scope and Application For Water Wastewater and Seawater 1 USEPA accepted for reporting wastewater analyses digestion required Procedure is equivalent to Standard Method 3500 Ni D for wastewater 2 Adapted from Chemie Analytique 36 43 1954 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 228 Instrument specific information Instrument Sample cell Cell orientation DR 6000 2495402 Fill line faces right DR 5000 2612602 Fill line faces user DR 3900 2612602 Fill line faces user DR 3800 DR 2800 DR 2700 2612602 Fill line faces right Before starting the test 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 Make the cotton plug pea size A larger plug will restrict the flow a smaller plug may become dislodged from the delivery tube of the funnel Chloroform D022 solutions are regulated as hazardous waste Do not pour these materials down the drain Water saturated with chlo2. a 300 mg L nickel standard by pipetting 15 mL of 1000 mg L Nickel standard into a 50 ml volumetric flask Dilute to volume and mix well Required for accuracy check Nickel Standard Solution 1000 mg L Ni Volumetric Pipet 15 mL Volumetric Flask 50 mL TenSette Pipet and tips Pipet Filler 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 Use the TenSette Pipet to prepare spiked samples add 0 2 mL 0 4 mL and 0 6 mL of 300 mg L standard to three 300 mL portions of fresh sample Follow the Heptoxime method for powder pillows test procedure for each of the spiked samples using the powder pillows starting with the 0 2 mL sample spike Measure each of the spiked samples in the instrument Select GRAPH to view the results Select IDEAL LINE or best fit to compare the standard addition results to the theoretical 100 recovery See Optional reagents and apparatus Nickel Page 4 of 6 Nickel Standard solution method Note Refer to the instrument user manual for specific software navigation instructions Required for accuracy check Nickel Standard Solution 1000 mg L Deionized water Volumetric fl
3. RING HACH COMPANY In the U S A Call toll free 800 227 4224 Outside the U S A Contact the HACH office or distributor serving you On the Worldwide Web www hach com E mail techhelp hach com Hach Company 2007 2010 2012 All rights reserved Printed in the U S A WORLD HEADQUARTERS Telephone 970 669 3050 FAX 970 669 2932 Edition 7
4. asks 500 mL and 1000 mL Volumetric pipets 10 mL and 50 mL Pipet filler Prepare a 10 0 mg L nickel working solution as follows a Pipet 10 0 mL of a Nickel Standard Solution 1000 mg L into a 1000 mL 1 liter volumetric flask b Dilute to the mark with deionized water Mix well Prepare this solution daily Prepare a 1 0 mg L nickel standard solution by diluting 50 0 mL of the 10 mg L working standard solution to 500 mL in a volumetric flask Use the standard solution in place of the sample Follow the Heptoxime 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 Method performance Precision Sensitivity Program Standard 95 Confidence Limits of Concentration change Distribution per 0 010 Abs change 335 1 00 mg L Ni 0 93 1 07 mg L Ni 0 02 mg L Ni Summary of method Nickel ion reacts with heptoxime to form a yellow colored complex which is then extracted into chloroform to concentrate the color and enable a more sensitive determination Chelating agents are added to the sample to overcome the interferences caused by cobalt copper and iron Readings are taken at 430 nm Consumables and
5. cts The final volume will be about 25 mL due to the slight solubility of chloroform in water 16 Wipe the prepared sample and insert it into the cell holder READ the results in mg L Ni Cobalt copper and iron interferences can be overcome by adding additional Nickel 1 Reagent Powder Pillows in step 3 of the Heptoxime method for powder pillows The tolerance limits of these interferences are shown in the nterfering substances table A preliminary acid digestion is required to determine any suspended or precipitated nickel and to eliminate interference by organic matter To eliminate this interference or to determine total recoverable nickel perform the USEPA approved digestion Nickel Page 3 of 6 Nickel Table 229 Interfering substances Pillows of Nickel 1 Tolerance Limit mg L Reagent Cobalt Couper iron 1 1 10 20 2 7 16 65 3 13 22 110 4 18 28 155 3 25 35 200 Sample collection preservation and storage Collect samples in acid washed plastic bottles Adjust the sample pH to 2 or less with Nitric Acid about 5 mL per liter Preserved samples can be stored up to six months at room temperature Before analysis adjust the sample pH to between 3 8 with 5 0 N Sodium Hydroxide Standard Solution Do not exceed pH 8 as this may cause some loss of nickel as a precipitate Correct the test results for volume additions Accuracy check Standard additions method sample spike Prepare
6. ime will begin Nickel Page 2 of 6 D i 05 00 a 4 Start the instrument timer 3 Add the contents of one Nickel 1 Reagent Powder Pillow to the funnel Stopper and invert to mix 7 When the timer expires add 10 mL of chloroform Insert the stopper and invert gently With the funnel inverted and the tip pointed away from people open the stopcock to vent A five minute reaction time will begin NNNMNN LIL I HRS MIN SEC 8 Close the stopcock and invert for 30 seconds Heptoxime method for powder pillows continued Nickel Ea 05 00 9 Start the instrument timer A third five minute reaction period will begin Invert the funnel several times over the five minute period 13 Blank Preparation Fill a second sample cell with 10 mL of chloroform Cap the cell Interferences 10 Prepared Sample When the timer expires wait for the layers to separate Insert a pea sized cotton plug into the delivery tube of the funnel Remove the stopper and drain the chloroform layer bottom layer into a sample cell Insert the stopper into the funnel 11 Repeat steps 7 through 10 two additional times with 10 mL volumes of chloroform The five minute reaction period is not necessary Zero 15 ZERO the instrument The display will show 0 00 mg L Ni 14 Wipe the blank and insert it into the cell holder 12 Cap the sample cell and invert to mix the extra
7. replacement items Required reagents Description Quantity Test Unit Catalog number Nickel Reagent Set 50 Tests includes 2243500 3 Chloroform ACS 30 mL 500 mL 1445849 2 Nickel 1 Reagent Powder Pillows 1 25 pkg 212368 2 Nickel 2 Reagent Powder Pillows 1 25 pkg 212468 Nickel Page 5 of 6 Nickel Required apparatus Description Quantity Unit Catalog number Clippers 1 each 96800 Cotton Balls absorbent 1 100 pkg 257201 Cylinder graduated 10 mL 1 each 50838 Cylinder graduated 500 mL 1 each 50849 Funnel separatory 500 mL 1 each 52049 Ring support 4 inch 1 each 58001 Sample Cell 1 inch square w stopper matched pair 2 2 pkg 2612602 Stand support 5 x 8 inch base 1 each 56300 Recommended standards Description Unit Catalog number Nickel Standard Solution 1000 mg L Ni NIST 100 mL 1417642 Water deionized 4L 27256 Optional reagents and apparatus Description Unit Catalog number Cylinder mixing 25 mL each 189640 Pipet volumetric Class A 15 mL each 1451539 Pipet Volumetric Class A 50 mL each 1451541 Flask Volumetric Class A 500 mL each 1457449 Flask Volumetric Class A 1000 mL each 1457453 Flask Volumetric Class A 50 mL each 1457441 Pipet Filler Safety Bulb each 1465100 Nitric Acid 1 1 500 mL 254049 Sodium Hydroxide Standard Solution 5 0 N 100 mL 245053 Pipet volumetric 10 mL each 1451538 FOR TECHNICAL ASSISTANCE PRICE INFORMATION AND ORDE
8. roform chloroform solutions and the cotton plug used in the delivery tube of the separatory funnel should be collected for proper disposal Refer to a current MSDS for safe handling and disposal instructions In bright light conditions e g direct sunlight it may be necessary to close the DR 3900 DR 3800 DR 2800 and DR 2700 cell compartment with the protective cover during measurements Collect the following items Description Quantity Chloroform ACS 30 mL Nickel 1 Reagent Powder Pillow 1 Nickel 2 Reagent Powder Pillow 1 Nickel Page 1 of 6 Nickel Collect the following items continued Description Quantity Clippers for Opening Pillows Cotton Balls Cylinder graduated 10 mL Cylinder graduated 500 mL Funnel separatory with stand and stopper Sample Cells see nstrument specific information 1 varies 1 1 1 See Consumables and replacement items for reorder information Heptoxime method for powder pillows Stored Programs 335 Nickel Heptoxime Start 2 Measure 300 mL of sample in a 500 mL graduated cylinder Pour into a 500 mL separatory funnel 1 Select the test Insert an adapter if required see nstrument specific information OK 05 00 6 Start the instrument timer 5 When the timer expires add the contents of one Nickel 2 Reagent Powder Pillow to the funnel Stopper and invert to mix A second five minute reaction t
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