Extract from manual:
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U. S. Environmental Protection Agency. 1983.
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Potassium: Method 258.1 (atomic absorption, direct aspiration). pp.
258.1-1 -- 258.1-2. In Methods for Chemical Analysis of Water and
Wastes, EPA-600/4-79-020. U.S.E.P.A., Cincinnati, Ohio, USA.
POTASSIUM
Method 258.1 (Atomic Absorption, direct aspiration)
STORET NO. Total 00937
Dissolved 00935
Suspended 00936
Optimum Concentration Range: 0.1-2 mg/1 using a wavelength of 766.5 nm
Sensitivity: 0.04 mg/l
Detection Limit: 0.01 mg/l
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Preparation of Standard Solution
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1. Stock Solution: Dissolve 0.1907 g of KCI (analytical reagent grade),
dried at 110 deg. C, in deionized distilled water and make up to 1
liter. 1 ml = 0.10 mg K( 1OO mg/l).
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2. Prepare dilutions of the stock solution to be used as calibration
standards at the time of analysis. The calibration standards should be
prepared using the same type of acid and at the same concentration as
will result in the sample to be analyzed either directly or after
processing.
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Sample Preservation
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1. For sample handling and preservation, see
[part 4.1] of the Atomic Absorption Methods section of this manual.
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Sample Preparation
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1. For the analysis of total potassium in domestic and industrial
effluents, the procedures for the determination of total metals as given
in [parts 4.1.3 and 4.1.4] of the Atomic
Absorption Methods section of this manual have been found to be
satisfactory.
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2. For ambient waters, a representative aliquot of a well mixed sample
may also be used directly for analysis. If suspended solids are present
in sufficient amounts to clog the nebulizer, the sample may be allowed
to settle and the supernatant liquid analyzed directly.
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Instrumental Parameters (General)
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1. Potassium hollow cathode lamp
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2. Wavelength: 766.5 nm
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3. Fuel: Acetylene
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4. Oxidant: Air
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5. Type of flame: Slightly oxidizing
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Analysis Procedure
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1. For the analysis procedure and the calculation, see "Direct
Aspiration", [part 9.1] of the Atomic
Absorption Methods section of this manual.
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Notes
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1. In air-acetylene or other high temperature flames ( >2800 deg. C),
potassium can experience partial ionization which indirectly affects
absorption sensitivity. The presence of other alkali salts in the sample
can reduce this ionization and thereby enhance analytical results. The
ionization suppressive effect of sodium is small if the ratio of Na to K
is under 10. Any enhancement due to sodium can be stabilized by adding
excess sodium (1000 ug/ml) to both sample and standard solutions. If
more stringent control of ionization is required, the addition of cesium
should be considered. Reagent blanks should be analyzed to correct for
potassium impurities in the buffer stock.
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2. The 404.4 nm line may also be used. This line has a relative
sensitivity of 500.
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3. To cover the range of potassium values normally observed in surface
waters (0.1-20 mg/l), it is suggested that the burner head be rotated. A
90 degree rotation of the burner head provides approximately one-eighth
the normal sensitivity.
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4. The flame photometric or calorimetric methods may also be used
(Standard Methods, 14th Edition, p 234 & 235).
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5. Data to be entered into STORET must be reported as mg/l.
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Precision and Accuracy
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1. In a single laboratory (EMSL), using distilled water samples spiked
at concentrations of 1.6 and 6.3 mg K/l. The standard deviations were
+/- 0.2 and +/-0.5, respectively. Recoveries at these levels were 103% and
102%, respectively.