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37

Known Subtraction

In the Known Subtraction method, a sample is measured with an ISE before and after the addition of a known
volume of a reactant standard. The reactant standard reacts with the measured Ion in the sample, reducing it’s
concentration. The mV difference is then used to calculate the concentration of the Ion in the original sample. The
stoichiometric ratio between Reactant Standard and Ion in the sample must be known.

Analyte Addition

Analyte Addition is similar to the Known Addition method, with the difference being that an aliquot of sample is
added to a known volume of standard. Both solutions contain the same measured Ion. The standard is measured
with an ISE before and after the addition of a known volume of a sample. The Ion concentration is then calculated
using the difference in mV potential. The sample should increase the concentration of the Ion being measured.

Analyte Subtraction

In the Analyte Subtraction method, an aliquot of sample is added to a reactant standard of known concentration
and volume. The sample partially reacts with the measured Ion. The stoichiometric ratio between standard and
sample must be known. The Ion concentration is then calculated using the difference in mV potential.

To set the Reading Mode:

• Press 

 while in 

ISE Measure

 mode.

• Press 

.

• Use 

 or 

 to select the Reading Mode option.

• Press 

 and use 

 or 

 to highlight the

desired option.

• Press 

 to confirm your selection or press 

 

to

cancel operation.

44

pH CALIBRATION

Calibrate the instrument often, especially if high accuracy is required.
The instrument should be recalibrated:
• Whenever the pH electrode is replaced.
• At least once a week.
• After testing aggressive chemicals.
• When “

Electrode Cond. Unknown

”, “

pH x Default Calibration

” or “

pH x Calibration Expired

message appears on the LCD, in the Reminder messages area. The “

x

” represents channel “

1

” or channel ”

2

”.

PREPARATION

Pour small quantities of the buffer solutions into clean beakers. If possible, use plastic beakers to minimize
any EMC interferences.
For accurate calibration and to minimize cross-contamination, use two beakers for each buffer solution. One
for rinsing the electrode and one for calibration.
If you are measuring in the acidic range, use pH 7.01 or 6.86 as first buffer and pH 4.01, 3.00 or 1.68
as second buffer. If you are measuring in the alkaline range, use pH 7.01 or 6.86 as first buffer and pH
10.01/9.18 or 12.45 as second buffer.
For extended range measurements (acidic and alkaline), perform a five points calibration by selecting five
of the available buffers.

CALIBRATION PROCEDURE

There are 8 standard pH buffers that are temperature-compensated during pH calibrations: 1.68, 3.00,
4.01, 6.86, 7.01, 9.18, 10.01 and 12.45. The standard pH buffers are temperature compensated during
calibration. Custom buffers require the user to use the actual buffer value at the temperature of use.
A minimum of a two point calibration using the standard pH buffers is required to determine the pH
electrode condition. The buffers should bracket the sample measurement pH.
An extended pH measurement range will require calibration at multiple points. The meter is able of
calibration with 5 pH buffers. For improved measurement accuracy, perform a multiple buffer calibration
bracketing and including the pH range the sample measurements.
The buffer group that will be available during calibration was set in pH setup 

 Calibration Buffer Entry

Type. The following example demonstrates pH electrode calibration if Manual selection was selected. In this
case all of the 8 standard buffers will be available for calibration.

Summary of Contents for HI 5221

Page 1: ...i n s t c o m MAN5222 02 15 PrintedinROMANIA Hanna Instruments Inc Highland Industrial Park 584 Park East Drive Woonsocket RI 02895 USA Technical Support for Customers Tel 800 426 6287 Fax 401 765 757...

Page 2: ...e mail us at tech hannainst com or view our worldwide contact list at www hannainst com WARRANTY All rights are reserved Reproduction in whole or in part is prohibited without the written consent of t...

Page 3: ...king material and examine it carefully to make sure that no damage has occurred during shipping If there is any damage notify your Dealer or the nearest Hanna Customer Service Center PRELIMINARY EXAMI...

Page 4: ...HI 5222 same for each measurement channel Log files include GLP information Basic Measurement can be viewed with detailed GLP information or with a Graph or a Log History User friendly interface on la...

Page 5: ...age Profile feature store up to ten different user setup HI 5222 five on each channel 76 HI 2031B Glass body semimicro conical refillable combination pH electrode Use semisolid products HI 1332B Plast...

Page 6: ...nnel 2 10 Temperature probe socket Channel 2 11 BNC electrode connector for pH ORP ISE measurements Channel 2 REAR PANEL 75 HI 1131B Glass body refillable double junction combination pH electrode Use...

Page 7: ...eral information about the selected option operation 74 ORP SOLUTIONS HI 7020L Test Solution 200 275 mV 500 mL bottle HI 7021L Test Solution 240 mV 500 mL bottle HI 7022L Test Solution 470 mV 500 mL b...

Page 8: ...p m I t u p n I 0 1 2 1 s m h o y a l p s i D s l e x i p 0 2 3 x 0 4 2 D C L c i h p a r G r o l o C y l p p u S r e w o P r e t p a d a c d V 2 1 t n e m o r i v n E g n i s n e d n o c n o n H R 5...

Page 9: ...utton located on the rear panel of the instrument Please wait until the instrument finishes the initialization process Note It is normal for the loading process to take a few seconds If the instrument...

Page 10: ...n i e r a n o i t c n u j e c n e r e f e r e h t n i s i e l p m a s e h t e r u s e k a M e h t k c e h C e g n a r d e i f i c e p s l a r e n e g e h t d n a l e v e l e t y l o r t c e l e E S I...

Page 11: ...r a faster response and to avoid cross contamination of the samples rinse the electrode tip with a few drops of the solution to be tested before taking measurements STORAGE PROCEDURE To minimize clogg...

Page 12: ...he protective cap off the pH electrode SALT DEPOSITS MAY BE PRESENT This is normal with electrodes They will disappear when rinsed with water During transport tiny bubbles of air may form inside the g...

Page 13: ...emperature During calibration the instrument will display the pH buffer value at 25 C P M E T S R E F F U B H p C K F 9 7 6 1 0 0 0 3 0 1 0 4 2 6 8 6 0 1 0 7 7 7 1 9 0 1 0 0 1 4 5 4 2 1 0 3 7 2 2 3 0...

Page 14: ...MP the sample concentration CSTD the standard concentration VSAMP the sample volume VSTD the standard volume VISA ISA volume E the difference of potential from the electrode S the electrode slope dete...

Page 15: ...adjustment is made to samples and standards Unknowns are measured directly by the instrument At lower concentrations in non linear regions of the electrode response multiple calibration points will e...

Page 16: ...e Press 65 ADDITIONAL INFORMATION ISE THEORY An Ion Selective Electrode ISE is an electrochemical sensor that changes voltage with the activity or concentration of ions in solutions The change in volt...

Page 17: ...ion Press and use key to highlight the desired parameter Use or to adjust the contrast backlight or to set the desired backlight saver time Press to confirm the modified options and return to the Syst...

Page 18: ...ss and then the desired parameter or HI 5222 only Only the selected measurement parameter lots will be displayed on the LCD Select the desired lot with or and press to display the logged data from the...

Page 19: ...meter reaches the stability criteria to go into Auto Hold mode The stored sample logs will be marked with an H to indicate the Auto Hold mode The virtual key returns operation to real time continuous...

Page 20: ...e r i D 2 l a u n a M g o L l a u n a M A N d l o H o t u A e l b a c i l p p A t o N 3 c i t a m o t u A g o L c i t a m o t u A d l o H o t u A t c e r i D 4 l a u n a M g o L l a u n a M 5 d l o H...

Page 21: ...p of the meter and ensures that the same procedure will be used To save the measurement configuration for pH mode Press and use or to highlight Profile Press to enable disable this feature pH SETUP 60...

Page 22: ...elect the Analyte Subtraction method see ISE Setup Reading Mode Prior to starting an AS procedure the ISE sensor must be calibrated with a minimum of two standards containing ISA The slope of the elec...

Page 23: ...he best results As a general rule the standard must be less concentrated than the sample so the addition of sample will increase the total Ion content of the beaker and change the mV value by at least...

Page 24: ...the observed mV Using a micropipet add a volume of the Reactant standard Start by adding 500 L at a time for example Watch the change in mV When you have observed approximately a 15 mV change from the...

Page 25: ...the solution and a mV value will show on the display Press to take the first mV reading When the reading is stable press to store the first mV reading The second step of the method will be displayed o...

Page 26: ...od Press and then to select ISE Measure mode for the selected channel Select the Known Addition method see ISE Setup for details Prior to starting a KA procedure the ISE sensor must be calibrated with...

Page 27: ...e of the incremental methods for measurement at least a two point ISE calibration must be performed to establish the electrode slope For accurate measurements add the appropriate ISA Ionic Strength Ad...

Page 28: ...oosing the AutoHold option the current reading can be frozen on the LCD when is pressed and the stability criterion is reached 53 If the isopotential point of the electrode is unknown the ISE calibrat...

Page 29: ...ared by pressing After 10 seconds will no longer be available Note It is very important to clear calibration history when a new electrode is used because most errors and warning messages that appear d...

Page 30: ...BRATION HI 5222 only For greater accuracy it is recommended to calibrate the ISE sensors frequently The instrument should be recalibrated when ISE x Calibration Expired the x represents channel 1 or c...

Page 31: ...larm State Press while in pH Measure mode Press Use or to select the Alarm option Press anduse or tohighlighttheAlarm State option Press anduse or tohighlightthedesired option Press to confirm your se...

Page 32: ...UREMENTS mV ORP MEASUREMENTS Oxidation reduction potential ORP measurements provide the quantification of the oxidizing or reducing power of the tested sample To correctly perform a redox measurement...

Page 33: ...le solution The pH reading is affected by temperature In order to measure the pH accurately the temperature effect must be compensated To use the Automatic Temperature Compensation ATC feature connect...

Page 34: ...for HI 5222 Select the Direct reading mode see pH Setup for details Place the electrode tip and the temperature probe approximately 4 cm 1 5 into the sample to be tested Allow time for the electrode...

Page 35: ...value can be adjusted using or Press to save the new temperature value If using Custom buffers press after buffer has been accepted to change actual buffer conditions A pop up menu will be displayed o...

Page 36: ...ctive nature of stability Known Addition In the Known Addition method a sample is measured with an ISE before and after the addition of a known volume of a standard The mV difference is then used to c...

Page 37: ...trode Cond Unknown pH x Default Calibration or pH x Calibration Expired message appears on the LCD in the Reminder messages area The x represents channel 1 or channel 2 PREPARATION Pour small quantiti...

Page 38: ...benefit from temperature compensated corrections if standards and sample temperatures differ from each other the Isopotential Point of the ISE is known If sample and standards are made at the same tem...

Page 39: ...key to select the next custom standard to be set Press to return to Edit Custom Standard options 42 To select the appropriate Ion Charge Slope use or and then press If the Ion electric charge is None...

Page 40: ...n constants Name Molar Weight and Electric Charge Slope while for the custom ISE all these constants can be manually set 41 To set the Electrode Type Press while in ISE Measure mode Press Use or to se...

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