Manual - Hach Chlorophosphonazo Indicator Solution
Contents
1. Interferences Table 164 Interfering substances Interfering substance Interference level Aluminum Negative interference above 150 ug L Ammonium No interference at or below 1000 pg L Copper Positive interference above 250 ug L Formaldehyde No interference at or below 47 000 ug L Potassium No interference at or below 1000 ug L Silicon Positive interference above 1000 ug L Sodium Negative interference above 79 000 pg L Treating analysis labware Clean all containers used in this test thoroughly to remove any traces of calcium or magnesium If possible use plastic containers for all analysis and storage Clean containers by normal means then rinse with ultra pure aldehyde free water Fill and soak for 10 minutes with a 1 25 dilution of Chlorophosphonazo Reagent in ultra pure water Rinse well with ultra pure water Keep containers tightly closed and dedicate them for ULR Hardness only If containers are rinsed and capped after each use only occasional soaking is necessary Fill the Pour Thru cell with this same mixture of chlorophosphonazo and water and let stand for several minutes Rinse with ultra pure water Avoid contamination of the Chlorophosphonazo Reagent bottle when placing the Repipet dispenser on the bottle Rinse the inlet tubing and inside of the dispenser cap with copious amounts of ultra pure water using a wash bottle Place the inlet tubing into a beaker of ultra pure water and depress the plunger 10 15 times t2. Hardness Total DOC316 53 01045 Calcium and Magnesium Chlorophosphonazo Rapid Liquid Method ULR 4 to 1000 ug L Ca and Mg as CaCO Pour Thru Cell Scope and Application For boiler and ultra pure water Method 8374 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 163 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 Before starting the test Pre clean the Pour Thru Cell and all labware as specified in Treating analysis labware For the most accurate magnesium test results keep the sample temperature between 21 29 C 70 84 F The test will detect any calcium or magnesium contamination in the mixing cylinder measuring droppers or sample cells To test cleanliness repeat the test until results are consistent Protect the Pour Thru Cell from contamination when not in use by inverting a small beaker over the top of the glass funnel If the sample concentration is greater than 750 pg
3. L a 1 1 dilution of the sample is recommended for greatest accuracy Use ultra pure aldehyde free water for the dilution Repeat the analysis on the diluted sample and multiply the resulting concentration by two Alternate forms should only be used when the sample is known to contain only Mg or Ca This method does not distinguish between the two forms Refer to the instrument User Manual for Pour Thru cell and module assembly and installation Use dedicated plasticware for this analysis In bright light conditions e g direct sunlight it may be necessary to close the DR 2800 or DR 2700 cell compartment with the protective cover during measurements Total hardness in mg L equals mg L Ca as CaCO plus mg L Mg as CaCO3 Ensure the pour thru cell is completely seated in the sample cell compartment Hardness Total Page 1 of 6 Hardness Total Collect the following items Description Quantity Chlorophosphonazo Indicator Solution 2mL CDTA Reagent for Ultra Low Range Hardness 1 drop Water Ultra pure Varies Cylinder graduated 50 mL poly 1 Dispenser Adjustable Volume 1 Flask Erlenmeyer PMP w cap 125 mL 1 Pour Thru Cell Module see nstrument specific information table 1 See Consumables and replacement items for reorder information Chlorophosphonazo rapid liquid method Stored Programs 227 Hardness Tot RL ULR Start 1 Select the test Insert an adapter if required nstrument specific
4. accepted the unspiked sample reading will appear in the top row See the user manual for more information 5 Use the TenSette Pipet to prepare spiked samples add 0 2 mL 0 4 mL and 0 6 mL of the prepared 20 000 ug L standard to three 50 mL portions of fresh sample 6 Follow the test procedure for each of the spiked samples starting with the 0 2 mL sample spike Measure each of the spiked samples in the instrument 7 Select GRAPH to view the results Select IDEAL LINE or best fit to compare the standard addition results to the theoretical 100 recovery Standard solution method Note Refer to the instrument user manual for specific software navigation instructions 1 Using a 0 50 mg L 500 ug L as CaCO3 Calcium Chloride Standard Solution perform the procedure using the standard in place of the sample 2 To adjust the calibration curve using the reading obtained with the 0 50 mg L Standard Solution select Options gt More gt Standard Adjust from the instrument menu 3 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 227 0 500 mg L Cr 495 505 ug L 8ug L Ca Summary of method Calcium and magnesium combine equivalently with the Chlorophospho
5. information 2 Flush the Pour Thru Cell with 50 mL of ultra pure water 6 Pour the contents of the 50 mL cylinder back into the flask 5 Fill the rinsed cylinder to the 50 mL mark with sample from the flask Discard remaining contents of the flask Hardness Total Page 2 of 6 H oN 3 Filla clean 125 mL plastic Erlenmeyer flask to overflowing with sample 4 Rinse a clean 50 mL plastic graduated cylinder three times with sample oo Collect sample directly in the flask if possible 7 Add 2 0 mL of Chlorophosphonazo Reagent to the sample with the Dispenser Swirl to mix 8 Pour approximately half 25 mL of the sample into the Pour Thru Cell Use a clean dry plastic 25 mL graduated cylinder to measure the sample Hardness Total Chlorophosphonazo rapid liquid method continued 3 Ne Zero Read 9 After the flow stops 10 Add one drop of CDTA 11 Pour the remaining 12 READ the results in ZERO the instrument Reagent for Ultra Low sample into the ug L CaCO The display will show Range Hardness to the Pour Thru Cell remaining sample in the 0 pg L CaCO3 flask Swirl to mix Complete steps 11 and 12 within one to two minutes 13 Using a wash bottle rinse the Pour Thru Cell with at least 75 mL of ultra pure water immediately after use Rinse the flask with ultra pure water Cap when finished Hardness Total Page 3 of 6 Hardness Total
6. 24 Hach Company 2007 2010 2012 All rights reserved Printed in the U S A 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 WORLD HEADQUARTERS Telephone 970 669 3050 FAX 970 669 2932 Edition 7
7. nazo Indicator to form a colored complex which absorbs light very strongly at 669 nm One drop of the CDTA reagent breaks up this complex and the resultant decrease in color is proportional to the amount of calcium and magnesium as CaCO3 in the sample Test results are measured at 669 nm Consumables and replacement items Required reagents Description Quantity Test Unit Catalog number Chlorophosphonazo Indicator Solution 2mL 500 mL 2589549 CDTA Reagent for Ultra Low Range Hardness 1 drop 10 mL SCDB 2589636 Required apparatus Description Quantity Unit Catalog number Cylinder graduated 50 mL poly 1 each 108141 Dispenser variable volume 1 each 2563137 Flask Erlenmeyer PMP w cap 125 mL 1 each 2089843 Hardness Total Page 5 of 6 Hardness Total Recommended standards Description Unit Catalog number Calcium Standard Solution 50 mg L as CaCO3 946 mL 2127716 Calcium Standard Solution 0 50 mg L as CaCO3 946 mL 2058016 Water ultra pure aldehyde free 500 mL 2594649 Optional reagents and apparatus Description Unit Catalog number Pipet TenSette 0 1 1 0 mL each 1970001 Pipet Tips for TenSette Pipet 1970001 50 pkg 2185696 Pipet volumetric Class A 20 mL each 1451520 Pipet filler Safety bulb each 1465100 Flask volumetric polypropylene 50 mL each 1406041 FOR TECHNICAL ASSISTANCE PRICE INFORMATION AND ORDERING HACH COMPANY In the U S A Call toll free 800 227 42
8. o rinse the inside of the dispenser For best results pour a small amount of reagent into the beaker of rinse water Remove the dispenser from the water and depress the plunger until all of the water has been expelled Shake off any excess water on the dispenser place the dispenser on the bottle and tighten Sample collection preservation and storage e Do not use glass containers e Collect samples in clean plastic containers preferably with screw type closures e Rinse containers several times with the water to be analyzed before collecting the final sample Seal to avoid contamination during transport Analyze as soon as possible Accuracy check Required for accuracy check e Calcium Chloride Standard Solution 50 mg L 50 000 ug L as CaCO3 TenSette Pipet and Pipet Tips Standard additions method sample spike 1 Prepare a 20 000 ug L 20 mg L CaCO standard by pipetting 20 mL of 50 mg L CaCO3 standard solution into a 50 mL plastic volumetric flask Dilute the solution with 50 mL of ultra pure water 2 After reading test results leave the sample cell unspiked sample in the instrument 3 Select Options gt More gt Standard Additions from the instrument menu Hardness Total Page 4 of 6 Hardness Total 4 Default values for standard concentration sample volume and spike volumes can be accepted or edited Accept the default values then read the unspiked sample measurement After values are
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