环境水中（类）金属及其化合物检测方案

Copper inSurface Fresh Water Copper inSurface Fresh Water Calibration and Analysis 1. Allow all the standards and the samples to attain room temperature for precise measurements since themeasurement is temperature sensitive. 2.Calibrate the meter using the 0.1 ppm followed by 1.0 ppm standard， stirring the standards at a gentleand uniform rate. 3. P1lace the electrode， temperature probe， and stirrer into the beaker with the 0.1 ppm standard suchthat the electrode tip ils faully。 immersed in the solution. The stirrer should be positioned slightlybelow the tip of the electrode. Press the STIRRER key on the meter to turn the stirrer on. Press theCALIBRATE key. 4. Wait for stable reading (1-2 minutes). Enter standard value of“0.10”using UP and DOWN arrowkeys and the DECIMAL/ DIGIT key. 5. Press the CALIBRATE key to accept 0.1 ppm standard and press the STIRRER key to turn thestirrer off. 6.Rinse electrode， temperature probe， and stirrer thoroughly with deionized water. Gently removeexcess solution from the outer sleeve of the electrode by dabbing with a clean paper tissue. Do notwipe or rub the sensing element. 7.Place the probes and stirrer into the beaker with the 1.0 ppm standard such that the electrode tip isfully immersed in the solution. Press the STIRRER key on the meter to turn the stirrer on. Wait for stable reading (1-2 minutes). Enter standard value of“1.00”using UP and DOWN arrowkeys and the DECIMAL/ DIGIT key. 9.Press the MEASURE key to accept 1 ppm standard and to move to the measure mode of the meter.Press the STIRRER key to turn the stirrer off. 10. Rinse electrode， temperature probe， and stirrer thoroughly with deionized water. Gently removeexcess solution from the outer sleeve of the electrode by dabbing with a clean paper tissue. Do notwipe or rub the sensing element of the electrode. 11. Place the probes and stirrer in a prepared sample such that the electrode tip is fully immersed in thesolution. Press the MEASURE key on the meter； the stirrer will turn on. The ISE：mg/L icon willflash as the measurement is being made. The ISE：mg/L icon will become solid and the display valuewill freeze when a stable reading is achieved. This value is logged and printed automatically and thestirrer turns off automatically. 12. Repeat steps 10 and 11 for additional samples. Upon completion or samples， rinse electrode with deionized water and store the electrode according toinstructions in the Electrode Storage section of this method note. Copper inSurface Fresh Water Introduction This method provides rapid， uncomplicated determinations of the free Cupric ions in Surface Fresh Water.The direct measurement of ions using ion selective electrodes is a well-established technique frequentlyused as a standard method of analysis， as a quality control step and to fulfill labeling requirements. Thisprocedure eliminates interferences associated with presence of color and solids. Recommended Equipment Cat.No. 3. Orion Benchtop Stirrer (or magnetic stir plate and bar) 096019 4. Orion benchtop electrode stand 1110001 5. Volumetric flask (1L， 100 mL) 6. Beakers (150 mL) 7. Volumetric Pipettes (1 mL， 10 mL) 8. Measuring Pipette (25 mL) 9. Graduated cylinder (100 mL) 3. ISA (Ionic Strength Adjustor) for cupric electrode 940011 3. Deionized water Calibration Standard Preparation 1.To prepare 100 ppm cupric stock standard， pipette 15.74 mL of the 0.1 M standard into a lLvolumetric flask. Dilute to the mark with deionized water. Mix well.1. 2.To prepare 1 ppm standard， pipette 1 mL of the 100 ppm cupric standard into a 100 ml volumetricflask. Dilute to the mark with deionized water. Mix well. 3.To prepare 0.1 ppm standard， pipette 10 mL of the 1 ppm cupric standard into a 100 ml volumetricflask. Dilute to the mark with deionized water. Mix well. 4.Transfer 100 mL of the 1 ppm standard into a beaker. Pipette 2 mL ISA. 5. Transfer 100 ml of the 0.1ppm standard into a beaker. Pipette 2 mL ISA. Sample Preparation 1.Adjust 600-700 mL sample to pH to 2-3 with concentrated nitric acid. 2e.Using a graduated cylinder， measure 100 mL of the sample into a beaker. Pipette 2 mL ISA. 3. Repeat this procedure for additional measurements. Five aliquots of surface fresh water were measured for copper. The obtained data in the table bellow. Surface fresh water ppm (mg/L) as Cu* Sample #1： 0.11 Sample #2： 919 Sample #3： 0.10 Sample #4： 0.11 Sample#5： 0.10 %CV Mean： 010Standard Deviation： 9.016.22 Electrode Storage The solution in the electrode should not be allowed to evaporate， causing crystallization. For short periods oftime (up to one week)， store the electrode in deionized water. For storage more than one week， drain the electrode， flush the inside with deionized water and store dry withthe cap on to protect the sensing element. Set Up Electrode Setup 1. Remove the rubber cap covering the electrode tip. 2. Fill outer chamber with Optimum Result""D filling solution. 3. Lift the filling solution bottle’s spout to a vertical position. 4 Insert the spout into the filling hole in the outer sleeve of the electrode and add a small amount of fillingsolution to the chamber. Then tip the electrode to moisten the o-ring at the top and return electrode to avertical position. 5. Holding the electrode by the barrel with one hand， use the thumb to push down on the electrode cap，allowing a few drops of filling solution to drain wetting the inner cone. 6. Release sleeve. If sleeve does not return to its original position immediately， check to see if the 0-ring ismoist enough and repeat steps 4-5 until the outer sleeve has returned to its original position. Add fillingsolution up to the fill hole. For initial meter setup please follow the steps in the Quick Start Guide which is attached to the meter itself.The Quick Start Guide also contains a layout of the meter keyboard for reference. Please note words in allcapitals such as POWER indicate a key on the meter， and words in quotations such as “Unit"indicate a displayon the meter screen. 1. Connect the electrode to the meter. 2. Connect the stirrer to the meter. 3. Press the POWER key on the meter to turn the meter on. 4. Note that the arrow on the left of the screen indicates the active line. If the top line is not active， press theLINE SELECTION key to change the selected line to the top line. Then press the UP or DOWN arrowkeys to change the measurement mode of the top line to ISE. 5. Press the SETUP key to enter ISE Setup. Press the LINE SELECTION key to select the bottom line.Press the UP or DOWN arrow keys to select“3”for“rES" which is an abbreviation for resolution ornumber of significant digits. Press the LINE SELECTION key to accept value. 6.Press the LINE SELECTION key to select the middle line， and press the DOWN arrow key to select“nLln”which is an abbreviation for non-linear blank correction. 7.Press the LINE SELECTION key to select the bottom line. Press UP or DOWN arrow keys to select“off”for “nLln". Press the LINE SELECTION key to accept value. 8.Press the LINE SELECTION key to select middle line， and press the DOWN arrow key to select “rAng”which is an abbreviation for measurement range. 9.Press the LINE SELECTION key to select the bottom line. Press the UP or DOWN arrow keys to select“HigH" for "rAng”. Press the LINE SELECTION key to accept value. 10. Press the LINE SELECTION key to select middle line， and press the DOWN arrow key to select “Unit". 11. Press the LINE SELECTION key to select the bottom line. Press the UP or DOWN arrow keys to select“mg/L”for“Unit". Press the LINE SELECTION key to accept value. 12. Press the MEASURE key to return to the measurement mode. If all steps were followed correctly the meter display will show three digits In the top line and“ISE： mg/L"tothe right of the top line. The meter and electrode are now ready for calibration. Note： The Orion Benchtop Stirrer must be turned on in General Instrument Setup before analysis， please see the QuickstartGuide for instructions. ofof