Manual - Hach Chlorine Reagent Set (Total)
Contents
1. Chlorine Total DOC316 53 01032 USEPA DPD Method Method 10014 ULR 2 to 500 ug L as Cl Pour Thru Cell and OriFlo Filtration Scope and Application For testing trace levels of chlorine and chloramines in treated domestic and industrial wastewater USEPA accepted for reporting for wastewater analysis 1 Adapted from Standard Methods for the Examination of Water and Wastewater 2 U S Patent 5 362 650 covers the procedure U S Patent 5 549 816 covers the OriFlo Filtration System 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 118 Instrument specific information Instrument Pour thru Kit Cell orientation Adapter DR 6000 LQV175 99 20002 Arrow faces right DR 5000 LZV479 DR 3900 LQV157 99 10002 Align cell flow arrows with arrows on cell compartment DR 3800 DR 2800 DR 2700 5940400 1 inch round path aligned with arrow on the adapter LZV585 B 1 Align for long path Before starting the test Analyze samples immediately Samples containing chlorine cannot be preserved for later analysis A reagent blank value for a combined lot of indicator buffer reagent solutions should be determined at least once a day If sample color or turbidity fluctuates frequently durin2. Interfering substance Interference levels and treatments Bromine Br Interferes at all levels Chlorine Dioxide ClO Interferes at all levels Chloramines organic May interfere Copper Cu2 Greater than 1000 ug L lodine l gt Interferes at all levels Adjust sample pH to 6 7 with 1 0 N Sulfuric Acid Add 9 drops Potassium lodide 30 g L to an 80 mL sample Manganese oxidized Mn4 Mix and wait 1 minute Mn or Chromium oxidized 4 Add 9 drops Sodium Arsenite 2 5 g L and mix Cr Analyze the treated sample as described in the procedure above Subtract the result of this test from the original analysis to obtain the correct concentration mg L nitrite Apparent ug L chlorine 7 2 0 mg L 3 pg L Nitrite NO uncommon in 5 0 mg L 5 ug L clean waters 10 0 mg L 7 ug L 15 0 mg L 16 pg L 20 0 mg L 18 ug L Ozone Interferes at all levels Peroxides o Peroxides ss May interfere May interfere Extreme sample pH or highly Adjust to pH 6 7 buffered samples 1 See Optional reagents and apparatus 2 Samples treated with sodium arsenite for interferences will be hazardous waste as regulated by the Federal RCRA for arsenic D004 Refer to the current MSDS for safe handling and disposal instructions Sample collection storage and preservation e Analyze samples for chlorine immediately after collection Chlorine is a strong oxidizing agent and it is unstable in natural waters It reacts rapidly
3. with various inorganic compounds and more slowly oxidizes organic compounds Many factors including reactant concentrations sunlight pH temperature and salinity influence decomposition of chlorine in water e Avoid plastic containers These may have a large chlorine demand e Pretreat glass sample containers to remove any chlorine demand by soaking in a dilute bleach solution 1 mL commercial bleach to 1 liter of deionized water for at least 1 hour e 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 e Acommon error in testing for chlorine is not obtaining a representative sample If sampling from a tap let the water flow for at least 5 minutes to ensure a representative sample Let the container overflow with the sample several times then cap the sample containers so there is no head space air above the sample Chlorine Total Page 7 of 10 Chlorine Total e Perform the chlorine analysis immediately Treating analysis labware Glassware used in this test must be chlorine demand free Fill the mixing cylinder and sample container with a dilute solution of chlorine bleach prepared by adding 1 mL of commercial bleach to 1 liter of water Soak in this solution at least one hour After soaking rinse thoroughly with deionized water and allow to dry before use Treat the Pour Thru Cell similarl
4. ULR and a clean tip to transfer DPD Indicator Solution for minutes Start the timer Chlorine Buffer Solution 1 0 mL of buffer from the Ultra Low Range Chlorine ampule a clean 50 mL mixing graduated cylinder Chlorine Total Page 5 of 10 Chlorine Total Determining the reagent blank value continued i 9 Use a TenSette Pipet and a clean tip to transfer 1 0 mL of indicator from the ampule to the cylinder Swirl to mix the reagents Proceed to step 10 within one minute Zero 13 When the flow stops ZERO the instrument The display will show 0 ug L Clo Chlorine Total Page 6 of 10 10 Fill the cylinder to the 50 mL mark with dechlorinated water from step 4 Cap and invert twice to mix Save the remaining water for step 12 14 When the timer expires pour the contents of the cylinder into the Pour Thru Cell results in ug L chlorine READ the aa 00 11 Start the instrument timer A three minute reaction time will begin 15 Use this value to correct the sample result obtained in this procedure See the user manual for details on saving the reagent blank value Ai 12 During the reaction period flush the Pour Thru Cell with the remainder of original dechlorinated water from step 10 16 Flush the Pour Thru Cell with at least 50 mL of deionized water immediately after use Chlorine Total Interferences Table 119 Interfering substances and levels
5. arting with the 0 1 mL sample spike Accept each standard additions reading by pressing READ Each addition should reflect approximately 100 recovery 7 After completing the sequence press GRAPH to view the best fit line through the standard additions data points accounting for the matrix interferences Press IDEAL LINE to view the relationship between the sample spikes and the Ideal Line of 100 recovery See Optional reagents and apparatus Chlorine Total Page 8 of 10 Chlorine Total Method performance Sensitivity Precision Concentration change Program Standard 95 Confidence Limits of per 0 010 Abs change Distribution Summary of method Several modifications to the normal DPD chlorine method are necessary to measure trace levels of chlorine The Pour Thru Cell must be used in the spectrophotometer Liquid reagents are also required The reproducible optics of the Pour Thru Cell give more stable readings than is possible with movable sample cells resulting in more stable measurements It is essential that interfering sample turbidity is removed using a 3 micron membrane filter To avoid chlorine loss the filtration is done after reacting the DPD with the chlorine in the sample The filter used has been specifically selected to avoid retention of the colored product Sample color is compensated by zeroing the spectrophotometer on a filtered sample The reagents are packaged in ampules and sealed under argon gas t
6. g the day determine a reagent blank for each sample Refer to Treating Analysis Labware on page 7 The reagent blank value is normally less than 5 ug L If the value is greater than 5 ug L an interfering substance may be present in the blanking water or the DPD Indicator may be degrading If there is doubt about the reagents repeat the reagent blank determination using chlorine demand free water for the sample Blanks up to 5 ug L may be used Use a new filter for each test Using an unspecified filter may give low analysis results or inability to filter the required volume Ampules contain more than 1 0 mL of solution for ease of transfer Discard excess reagent in the ampule Refer to the instrument User Manual for Pour Thru cell and module assembly and installation Protect the Pour Thru Cell from contamination when not in use by inverting a small beaker over the top of the glass funnel Use forceps to handle filters Make sure the Pour Thru cell is completely seated in the sample cell compartment Chlorine Total Page 1 of 10 Chlorine Total Collect the following items Description Quantity ULR Chlorine Buffer Solution 1 5 mL ampules 1 mL DPD Indicator Solution for ULR Chlorine 1 5 mL ampules 1 mL Blanking Reagent for ULR Chlorine 1 mL Membrane Filters 3 micron 25 mm 1 OriFlo Assembly 1 Beaker 250 mL 1 Cylinder graduated mixing 50 mL 1 Pipet TenSette 0 1 to 1 0 mL 1 Pipet Tips 2 Deionized water Varies Ampu
7. le Breaker 1 Pour Thru Module and cell 1 See Consumables and replacement items for reorder information DPD method for Pour Thru Cell a Stored Programs Start 1 Select the test 2 Flush the Pour Thru 3 Unscrew the cap from 4 Install anew 3 micron Insert an adapter if cell with 50 mL of the OriFlo plunger filter white into the cap deionized water assembly Be sure thatthe well Wet the filter with a required nstrument specific information O ring is properly seated few drops of deionized in the cap water Reassemble and hand tighten the cap onto the plunger Chlorine Total Page 2 of 10 DPD method for Pour Thru Cell continued Chlorine Total 5 Open one ULR Chlorine Buffer Solution Ampule 9 Prepared Sample Avoiding extra agitation carefully fill the cylinder to the 50 mL mark with sample Stopper the cylinder Gently invert it twice to mix ER 6 Using a TenSette Pipet and a clean tip transfer 1 0 mL of buffer from the ampule to a clean treated 50 mL graduated mixing cylinder OK 03 00 10 Press TIMER gt OK A three minute reaction time will begin Perform steps 11 16 during this period Measure the reacted sample 3 6 minutes after mixing the sample and reagents If less than three minutes elapses the reaction with chloramines may be incomplete A reading after six minutes may result in higher reagent blank values 7 Open one ampule of DPD Indica
8. ltered sample A new membrane may be required for very turbid samples Alternatively use a second Quick Filter unit with anew membrane filter installed 20 Flush the Pour Thru Cell with at least 50 mL of deionized water immediately after use 19 Pour the filtered reacted sample from the plunger reservoir into the Pour Thru Cell READ the results in ug L chlorine If a dechlorinating agent e g Sulfite or sulfur dioxide is present the sample result corrected for the reagent blank will read 0 or a slightly negative value Subtract the reagent blank value See Determining the reagent blank value from the sample value obtained in step 19 Chlorine Total Determining the reagent blank value g Stored Programs 86 Chlorine Total ULR Start M 1 Select the test 2 Install the Pour Thru 3 Collect about100 mL 4 Use a TenSette Pipet Make sure that the reagent module of deionized or tap water to add 1 0 mL of Blanking blank setting is off Flush the Pour Thru cell in aclean 250 mL beaker Reagent to the beaker San heueermanoaiior with 50 mL of deionized Swirl several times to mix information water The Blanking Reagent removes chlorine and chloramines from the water Note The solution from step 4 will be used in Step 10 E 05 00 f 5 Access the general 6 Afterthe timer expires 7 Use a TenSette Pipet 8 Open one ampule of timer and set it for five open one ampule of
9. mpule 25 30 mg L 2 mL 20 pkg 2630020 Optional reagents and apparatus Description Unit Catalog number Forceps flat square tips 115 mm each 1453700 Potassium lodide 30 g L 100 mL MDB 34332 Sodium Arsenite 5 g L 100 mL 104732 Sulfuric Acid 1 N 100 mL 100 mL MDB 127032 Sulfuric Acid 5 25 N 1000 mL 244953 FOR TECHNICAL ASSISTANCE PRICE INFORMATION AND ORDERING Inthe 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 HACH COMPANY WORLD HEADQUARTERS Telephone 970 669 3050 FAX 970 669 2932 Edition 7
10. o ensure stability Use of liquid reagents eliminates any slight turbidity that might be caused by using powdered reagents Due to the possible oxidation of the reagents which could give a positive chlorine reading in the blank a reagent blank must be determined at least once a day for each lot of reagent used This reagent blank value is subtracted from the sample result and the corrected value is the actual chlorine concentration Test results are measured at 515 nm Chlorine Total Page 9 of 10 Chlorine Total Consumables and replacement items Required reagents Description Quantity Test Unit Catalog number ULR Chlorine Reagent Set approximately 20 tests includes 2563000 ULR Chlorine Buffer Solution 1 5 mL ampules 1 mL 20 pkg 2493120 DPD Indicator Solution for ULR Chlorine 1 5 mL ampules 1 mL 20 pkg 2493220 Blanking Reagent for ULR Chlorine 1 mL 29 mL 2493023 Water deionized varies 4L 27256 Required apparatus Description Quantity Unit Catalog number ULR Chlorine Apparatus Set includes 2595600 Membrane Filters 3 micron 25 mm 1 25 pkg 2594025 OriFlo Assembly 1 each 4966000 Beaker 250 mL 1 each 50046H Breaker ampule 1 each 2484600 Cylinder graduated mixing 50 mL 1 each 189641 Pipet TenSette 0 1 to 1 0 mL 1 each 1970001 Pipet Tips for TenSette Pipet 1970001 2 50 pkg 2185696 Recommended standards Description Unit Catalog number Chlorine Standard Solution Voluette A
11. tor Solution for Ultra Low Range Chlorine 11 Push the valve button on the OriFlo barrel assembly in closed position Place the barrel assembly into its stand Pour approximately 50 mL of the original sample into the barrel The lower ring on the barrel assembly represents about a 50 mL volume 8 Use a TenSette Pipet and a Clean tip to transfer 1 0 mL of indicator from the ampule to the graduated mixing cylinder Swirl to mix Proceed to step 9 within one minute ie LI 12 Insert the plunger into the barrel and slowly push the plunger down with even pressure until the plunger is fully seated Chlorine Total Page 3 of 10 Chlorine Total DPD method for Pour Thru Cell continued Zero 13 Pour the filtered sample from the plunger reservoir into the Pour Thru Cell 14 When the flow stops ZERO the instrument The display will show 0 ug L Clo 17 When the timer expires pour the contents of the mixing cylinder into the barrel 18 Insert the plunger into the barrel and slowly push the plunger down with even pressure until the plunger is fully seated Chlorine Total Page 4 of 10 po 16 Push the barrel valve button to the closed position Place the barrel assembly into its stand 15 Pull the barrel valve button out to the open position Pull the plunger up to separate it from the barrel assembly Discard the remaining unfi
12. y with dilute bleach and let stand for several minutes Rinse several times with deionized water Cleaning the Pour Thru cell The Pour Thru Cell may accumulate a buildup of colored reaction products especially if the reacted solutions are allowed to remain in the cell for long periods after measurement Remove the buildup by rinsing the cell with 5 25 N Sulfuric Acid followed by several rinsings with deionized water Accuracy check Required for accuracy check e Low Range Chlorine Voluette Ampule Standard Solution 25 to 30 mg L 25 000 to 30 000 ug L Clo e TenSette Pipet and Pipet Tips e Ampule Breaker Standard additions method samples spike 1 After reading test results leave the sample cell unspiked sample in the instrument 2 Select Options gt More gt Standard Additions from the instrument menu 3 Default values for standard concentration sample volume and spike volumes can be accepted or edited Enter the chlorine concentration from the ampule package After values are accepted the unspiked sample reading will appear in the top row See the user manual for more information 4 Snap the top off a Low Range Chlorine Voluette Ampule Standard Solution 25 to 30 mg L 25 000 to 30 000 ug L 5 Prepare three sample spikes Use the TenSette Pipet to add 0 1 0 2 and 0 3 mL of standard to three 50 mL samples respectively Swirl gently to mix 6 Analyze each sample spike as described in the procedure above st
Download Pdf Manuals
Related Search