Chlorine, Total
Contents
1. Pull the barrel valve button out to the open position Pull the plunger up to separate it from the barrel assembly Discard the remaining unfiltered sample A new membrane may be required for very turbid samples Alternatively use a second Quick Filter unit with a new membrane filter installed 4 12 Insert the plunger into the barrel and slowly push the plunger down with even pressure until the plunger is fully seated a 16 Push the barrel valve button to the closed position Place the barrel assembly into its stand Chlorine Total Page 3 of 10 Chlorine Total ULR 2 to 500 pg L as Clo Boe 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 y Options Stored Programs 86 Chlorine Total ULR a Reagent Blank Off Start me 2 Make sure that the reagent blank setting is off Press OPTIONS gt MORE gt REAGENT BLANK gt SOFF See the user manual for information 1 Select the test Chlorine Total Page 4 of 10 Les L 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 Results are in pg L chlorine Subtract the reagent blank value Determining the Reagent2. in water Avoid plastic containers since these may have a large chlorine demand Pretreat glass sample containers to remove any chlorine demand by soaking in a dilute bleach solution 1 mL commercial bleach to liter of deionized water for 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 A common 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 Perform the chlorine analysis immediately Treating Analysis Labware Glassware used in this test must be chlorine demand free Fill the 100 mL 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 similarly 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
3. mg L 2 mL 20 pkg 26300 20 Optional Reagents and Apparatus Description Cat No Potassium lodide 30 g L 100 mL 343 32 Sodium Arsenite 5 g L 100 mL 1047 32 Sulfuric Acid 1 N 100 mL 1270 32 Sulfuric Acid 5 25 N 100 mL 2449 53 ChlorineTot_10014_ULR_RL_OriFlo fm Chlorine Total Page 9 of 10 FOR TECHNICAL ASSISTANCE PRICE INFORMATION AND ORDERING HACH COMPANY 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 On the Worldwide Web www hach com E mail techhelp hach com FAX 970 669 2932 Hach Company 2005 All rights reserved Printed in Germany Updated April 05 Edition 1
4. reagents are packaged in ampules and sealed under argon gas to 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 Consumables and Replacement Items Required Reagents Description Quantity Test Unit Cat No ULR Chlorine Reagent Set approximately 20 tests includes 25630 00 ULR Chlorine Buffer Solution 1 5 mL ampules 1 mL 20 pkg 24931 20 DPD Indicator Solution for ULR Chlorine 1 5 mL ampules 1 mL 20 pkg 24932 20 Blanking Reagent for ULR Chlorine 1 mL 29 mL LZV479 Required Apparatus Description Quantity Test Unit Cat No ULR Chlorine Apparatus Set includes 25956 00 Membrane Filters 3 micron 25 mm 1 25 pkg 25940 25 OriFlo Assembly 1 each 49660 00 Beaker 250 mL 1 each 500 46H Cylinder graduated mixing 50 mL 1 each 1896 41 Pipet TenSette 0 1 to 1 0 mL 1 each 19700 01 Pipet Tips for TenSette Pipet 19700 01 2 50 pkg 21856 96 Pour Thru Cell Module Kit 1 each 59122 00 Recommended Standards Description Unit Cat No Chlorine Standard Solution Voluette Ampule 25 30
5. Blank Value from the sample value obtained in step 19 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 p 4 Collect about 100 mL of deionized or tap water in a clean 250 mL beaker 3 Install the Pour Thru module and cell Flush the Pour Thru cell with 50 mL of deionized water ChlorineTot_10014_ULR_RL_OriFlo fm 5 Using a TenSette Pipet add 1 0 mL of Blanking Reagent to the beaker Swirl several times to mix The Blanking Reagent removes chlorine and chloramines from the water 9 Fill the cylinder to the 50 mL mark with dechlorinated water from step 5 Cap and invert twice to mix Save the remaining water for step 11 ChlorineTot_10014_ULR_RL_OriFlo fm a Options GENERAL TIMER 05 00 OK 6 Press OPTIONS gt MORE gt TIMER gt GENERAL TIMER Set a 5 minute timer and press OK A five minute dechlorination period will begin OK 03 00 10 Press TIMER gt OK A three minute reaction time will begin Chlorine Total ULR 2 to 500 pg L as Clo 7 After the timer expires break open one ampule of ULR Chlorine Buffer Solution Using a TenSette Pipet and clean tip transfer 1 0 mL of buffer from the ampule to a clean 50 mL mixing graduated cylinder 11 During the reaction period flush the Pour Thru Cell with the remainder of orig
6. Chlorine Total Method 10014 DPD Method Pour Thru Cell and OriFlo Filtration ULR 2 to 500 pg L as Cl Scope and Application For detecting trace levels of chlorine and chloramines in clean waters relatively free of color and turbidity USEPA accepted for reporting for wastewater analysis2 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 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 during 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 a
7. additions reading by pressing READ Each addition should reflect approximately 100 recovery 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 Method Performance Precision Standard 295 pg L Clo Program 95 Confidence Limits of Distribution 86 290 300 ug L Clo Sensitivity Portion of Curve AAbs AConcentration Entire range 0 010 17 pg L Clo Chlorine Total Page 8 of 10 ChlorineTot_10014_ULR_RL_OriFlo fm Chlorine Total ULR 2 to 500 pg L as Cl Summary of Method 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 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 The
8. de 30 g L to an 80 mL sample Add 9 drops Sodium Arsenite 2 5 g L and mix Analyze the treated sample as described in the procedure above Subtract the result of this test from the original analysis to obtain the correct Nitrite NO27 uncommon in clean waters mg L nitrite Apparent pg L chlorine 2 0 mg L 3 ug L 5 0 mg L 5 ug L 10 0 mg L 7 pg L 15 0 mg L 16 ug L 20 0 mg L 18 ug L Chlorine Total Page 6 of 10 ChlorineTot_10014_ULR_RL_OriFlo fm Chlorine Total ULR 2 to 500 pg L as Clo Table 1 Interfering Substances and Levels continued Interfering Substance Interference Levels and Treatments Ozone Interferes at all levels Peroxides May interfere Extreme sample pH or highly buffered samples Adjust taph 6 7 1 See Optional Reagents and Apparatus on page 9 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 Analyze samples for chlorine immediately after collection Chlorine is a strong oxidizing agent and it is unstable in natural waters It reacts rapidly with various inorganic compounds and more slowly oxidizes organic compounds Many factors including reactant concentrations sunlight pH temperature and salinity influence decomposition of chlorine
9. 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 See Optional Reagents and Apparatus on page 9 Chlorine Total ChlorineTot_10014_ULR_RL_OriFlo fm Page 7 of 10 Chlorine Total ULR 2 to 500 pg L as Clo Accuracy Check Standard Additions Method Sample Spike 1 2 After reading test results leave the sample cell unspiked sample in the instrument Press OPTIONS gt MORE Press STANDARD ADDITIONS A keypad will appear Enter the average chlorine concentration shown on the certificate enclosed with the chlorine voluette ampules Multiply the mg L value from the label by 1000 to enter this as pg L Press OK A summary of the Standard Additions procedure will appear Press OK to accept the values for standard concentration sample volume and spike volumes as shown Press Edit to change these values After values are accepted the unspiked sample reading will appear in the top row See the user manual for more information Snap the top off a Low Range Chlorine Voluette Ampule Standard Solution 25 to 30 mg L 25 000 to 30 000 pg L 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 Analyze each sample spike as described in the procedure above starting with the 0 1 mL sample spike Accept each standard
10. inal dechlorinated water from step 9 8 Break open one ampule of DPD Indicator Solution for Ultra Low Range Chlorine Using a TenSette Pipet and a clean tip transfer 1 0 mL of indicator from the ampule to the cylinder Swirl to mix the reagents Proceed to step 9 within one minute Zero 12 When the flow stops press ZERO The display will show 0 pg L Clo Chlorine Total Page 5 of 10 Chlorine Total ULR 2 to 500 pg L as Cl 13 When the timer expires introduce the contents of the cylinder into the Pour Thru Cell Results are in ug L chlorine Interferences OS Ca a eS Th Ca Coe Bone HEE EE E ES EI E EA 14 Use this value to correct the sample result obtained in this procedure See the user manual for details on saving the reagent blank value 15 Flush the Pour Thru Cell with at least 50 mL of deionized water immediately after use Table 1 Interfering Substances and Levels Interfering Substance Interference Levels and Treatments Bromine Bro Interferes at all levels Chlorine Dioxide ClO Interferes at all levels Chloramines organic May interfere Copper Cu2 Greater than 1000 pg L lodine lo Interferes at all levels Manganese oxidized Mn 4 Mn or Chromium oxidized Cro Mix and wait 1 minute or Se Nes concentration Adjust sample pH to 6 7 with 1 000 N Sulfuric Acid Add 9 drops Potassium lodi
11. micron filter into the cap well Wet the filter with a few drops of deionized water Reassemble and hand tighten the cap onto the plunger i 8 Using a TenSette Pipet and a clean tip transfer 1 0 mL of indicator from the ampule to the graduated mixing cylinder Swirl to mix Proceed to step 9 within one minute ChlorineTot_10014_ULR_RL_OriFlo fm O a 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 RU 13 Pour the filtered sample from the plunger reservoir into the Pour Thru Cell ChlorineTot_10014_ULR_RL_OriFlo fm Eee 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 Zero 14 When the flow stops press ZERO The display will show 0 pg L Clo Chlorine Total ULR 2 to 500 pg L as Clo i 11 Push the valve button on the OriFlo barrel assembly to the 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 N 1 15
12. mpule 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 Collect the following items 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 Pour Thru Module and cell 1 Note Reorder information for consumables and replacement items is on page 9 Chlorine Total ChlorineTot_10014_ULR_RL_OriFlo fm Page 1 of 10 Chlorine Total ULR 2 to 500 pg L as Cl Stored Programs 86 Chlorine Total ULR Start 1 Select the test 2 Install the Pour Thru module and cell 3 Unscrew the cap from the OriFlo plunger assembly Be sure that the O ring is properly seated in the cap Flush the Pour Thru cell with 50 mL of deionized water I 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 5 Break open one ULR Chlorine Buffer Solution Ampule 7 Break open one ampule of DPD Indicator Solution for Ultra Low Range Chlorine Chlorine Total Page 2 of 10 FILTER 4 Install a new 3
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