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DR/4000

PROCEDURE POTASSIUM
Method 8049 Tetraphenylborate Method
(0 to 7.0 mg/L)
Scope and Application: For water, wastewater and seawater.

HACH PROGRAM: ###


Potassium

1. If this test has not 2. The display will show: 3. Fill a mixing 4. Add the contents
been run on this USER PROGRAM: ### graduated cylinder with of one Potassium 1
instrument, perform the Potassium 25 mL of sample. Reagent Pillow. Add
User Programming Note: Filter highly colored or the contents of one
procedure under The wavelength (λ), turbid samples. Use filtered Potassium 2 Reagent
Calibration. 650 nm, is automatically sample here and in Step 8. Pillow. Stopper. Invert
selected. several times to mix.
Press the soft key under Note: ### refers to the
USER PROGRAM. Select number assigned during
the stored program calibration.
number for potassium (K)
using the numeric keys.
Press: ENTER
Note: If samples cannot be
analyzed immediately, see
Sample Collection,
Preservation and Storage
below.
Note: Because of potential
variation between lots of
Potassium 3 Reagent,
perform a new calibration for
each lot of reagent to obtain
best accuracy. Prepare and
store the calibration as
directed under Calibration
following these steps.
Note: The Flow Cell or
Sipper Cell Modules may not
be used for this procedure.

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30 seconds
START
TIMER

5. Add the contents of 6. Press the soft key 7. Pour the solution 8. When the timer beeps,
one Potassium 3 Reagent under START TIMER. from the cylinder into a fill the second sample cell
Pillow after the solution A 3-minute reaction 25-mL sample cell (the (the blank) with 25 mL
clears. Stopper. Shake for period will begin. prepared sample). of sample. Place it into
30 seconds. the cell holder. Close the
Note: A white turbidity will light shield.
form if potassium is present.

ZERO

9. Press the soft key 10. Within seven


under ZERO. minutes after the timer
The display will show: beeps, place the prepared
sample into the cell
0.0 mg/L K holder. Close the light
Note: For alternate shield. Results in mg/L
concentration units, potassium (or chosen
press the soft key under units) will be displayed.
OPTIONS. Then press the
soft key under UNITS to scroll Note: Clean the cells with
through the available soap and a brush.
options. Press ENTER to
return to the read screen.

POTASSIUM
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POTASSIUM, continued

Interferences
The substances listed below have been tested and will not interfere at or below
the levels stated. If these substances are present at higher levels, analysts need
to conduct interference studies at the higher levels to determine if the
substance interferes.

Interfering Substance Interference Levels and Treatments


Ammonium Nitrogen 15 mg/L as N
Calcium 7000 mg/L as CaCO3
Chloride 15,000 mg/L
Magnesium 6000 mg/L as CaCO3

Sample Collection, Preservation and Storage


Collect samples in acid-washed plastic bottles. Adjust the pH to 2 or less with
nitric acid (about 2 mL per liter). Preserved samples may be stored at least six
months at room temperature. Adjust the pH to 4–5 with 5.0 N Sodium Hydroxide
before analysis. Do not measure pH in the sample container with a pH electrode,
as this will introduce potassium from the filling solution. Use pH paper or pour off
sample and test pH in a separate beaker. Correct the test result for volume
additions; see Section 1.2.2 Correcting for Volume Additions.

Accuracy Check
Standard Additions Method

a. Leave the unspiked sample in the sample compartment. Verify that the
units displayed are in mg/L. Select standard additions mode by pressing
the soft keys under OPTIONS, (MORE) and then STD ADD.
b. Press ENTER to accept the default sample volume (mL), 25.
c. Press ENTER to accept the default standard concentration (mg/L), 250.
d. Press the soft key under ENTRY DONE.
e. Snap the neck off a Potassium Voluette Ampule Standard, 250-mg/L K.
f. Use the TenSette Pipet to add 0.1 mL, 0.2 mL and 0.3 mL of standard,
respectively to three 25-mL samples and mix each thoroughly.
g. Analyze each standard addition sample as described above. Accept
standard additions reading by pressing the soft key under READ each time.
Each addition should reflect approximately 100% recovery.
h. After completing the sequence, the display will show the extrapolated
concentration value and the “best-fit” line through the standard additions
data points, accounting for matrix interferences.
i. See Section 1.4.1 Standard Additions for more information.

Calibration
Prepare calibration standards containing 1, 2, 3, 4, 5, 6, 7, and 8 mg/L potassium
as follows:

a. Into eight different 100-mL Class A volumetric flasks, pipet 1.0, 2.0,
3.0, 4.0, 5.0, 6.0, 7.0 and 8.0 mL of the 100-mg/L Potassium Standard
Solution using class A glassware or TenSette Pipet.

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POTASSIUM, continued
b. Dilute to the mark with deionized water. Mix thoroughly.
c. Use deionized water for the 0-mg/L potassium standard.

User Programming

a. Start from the MAIN MENU. Press the soft key under USER PROGRAM.
b. If you have not performed a potassium calibration before, press the soft
key under CREATE. Key any available program number you wish to use for
potassium testing. Press ENTER. Press the soft key under COPY PROGRAM.
Select program number 3100 and press ENTER. If you already have a
working potassium program, press the soft key under EDIT, select the
program number and press ENTER.
c. Press the down arrow until you highlight the parameter Calib. table. Press
the soft key under EDIT TABLE. Press the up arrow to highlight the very
first concentration in the list. Press the soft key under EDIT ABS. Press CE
and then ENTER to erase the first, inaccurate, absorbance value. Repeat to
erase all the absorbance values. Press the soft key under ENTRY DONE.
Note: An approximate calibration curve is preprogrammed within Program 3100.
For improved accuracy, a new calibration should be performed with each new lot of
reagents.

d. Note which mg/L value is highlighted. Perform steps 3 through 7 of the


potassium Tetraphenylborate Method on a potassium standard of the
indicated concentration. Place a 25-mL sample cell containing only
deionized water into the cell holder and close the lid. Press the soft key
under ZERO. Place the prepared sample in the cell holder. Press the soft
key under READ to accept the absorbance value. Repeat this step for
each standard.
e. In the Curve fit: display, press the soft key under NEXT FORMULA until
C = a + bA + CA2 + dA3 is displayed. Press the soft key under FORCE O:
once to ON is selected. Press EXIT until Store Changes? is displayed. Press
the soft key under YES. The program is ready for use.
Note: Some variations of the calibration procedure are possible. See the DR/4000
Instrument Manual for details.

Summary of Method
Potassium in the sample reacts with sodium tetraphenylborate to form an
insoluble white solid. The amount of turbidity produced is proportional to the
potassium concentration.

Safety
Good safety habits and laboratory techniques should be used throughout the
procedure. Consult the Material Safety Data Sheet for information specific to the
reagents used. For additional information, refer to Section 1.

Pollution Prevention and Waste Management


The final samples are highly acidic. Neutralize to pH 6–9 and flush to drain for
disposal. For more information on pollution prevention and waste management,
refer to Section 1.

POTASSIUM
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REQUIRED REAGENTS AND STANDARDS


Potassium Reagent Set (100 tests) ..........................................................................................................24591-00
Includes: (4) 14321-98, (4) 14322-18, (1) 14323-99
Quantity Required
Description per test Unit Cat. No.
Potassium 1 Reagent Powder Pillows ............................................ 1 pillow.............. 25/pkg.................14321-98
Potassium 2 Reagent Powder Pillows ............................................ 1 pillow.............. 25/pkg.................14322-98
Potassium 3 Reagent Powder Pillows ............................................ 1 pillow............ 100/pkg.................14323-99
Potassium Standard Solution, 100-mg/L..........................................varies...............500 mL.................23517-49

REQUIRED EQUIPMENT AND SUPPLIES


Clippers, for opening powder pillows ..................................................1 ....................... each.....................968-00
Cylinder, mixing, graduated, 25-mL ....................................................1 ....................... each...................1896-40
DR/4000 1-inch Cell Adapter ..............................................................1 ....................... each.................48190-00
Flask, volumetric, 100-mL, Class A ....................................................8 ....................... each.................14574-42
Pipet, TenSette™, 1–10 mL .................................................................1 ....................... each.................19700-10
Pipet Tips, for 19700-10 TenSette™ Pipet.......................................varies................ 50/pkg.................21997-96

OPTIONAL REAGENTS AND STANDARDS


Nitric Acid, ACS .......................................................................................................500 mL.....................152-49
Nitric Acid Solution, 1:1 ...........................................................................................500 mL...................2540-49
Potassium Standard Solution, 5-mg/L.......................................................................500 mL.................20583-49
Potassium Standard Solution, 100-mg/L...................................................................100 mL.................22404-42
Potassium Standard Solution, 10-mL Voluette™ Ampule, 250-mg/L....................... 16/pkg.................14790-10
Sodium Hydroxide Standard Solution, 5.0 N....................................................... 59 mL DB...................2450-26
Water, deionized ......................................................................................................... 4 liters.....................272-56

OPTION EQUIPMENT AND SUPPLIES


DR/4000 Carousel Module............................................................................................. each.................48070-02
pH Paper, pH 1.0 to 11.0 ...................................................................................... 5 rolls/pkg.....................391-33
pH Meter, sension™1, portable.................................................................................... each.................51700-00

POTASSIUM
Potassium_PP_Other_TPB_Eng_4000.fm Page 5 of 6
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, 1997-2003. All rights reserved. Printed in the U.S.A. 6/03 11ed
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