SKALAR METHODS
ANALYSIS: POTASSIUM IN SOIL
ACCORDING TO:
GOST 26204-91 Chiricov method
5 - 500 mg K2O/kg
(≈ 0.2 - 20 mg K2O/liter)
GOST 26205-91 Machigin method
5 - 500 mg K2O/kg
(≈ 0.25 - 25 mg K2O/liter)
GOST 26207-91 Kirsanov method
1.25 - 125 mg K2O/kg
(≈ 0.25 - 25 mg K2O/liter)
SAN++
Catnr. 569-006 issue 071323/99400166
PRINCIPLE
The automated determination of Potassium is based on the following procedure; the sample is aspirated
into a flame. Potassium is measured at 776 nm.
LABORATORY FACILITIES
1. Maximum power consumption depending on the analyzer configuration, 2000 VA. Check voltage at the
back of the instrument before installation.
2. Facilities for chemical wastes. Check environmental regulations for proper disposal of waste.
PROCEDURE SAMPLE PREPARATION
Sample pretreatment
1. Dry soil to air-dried condition at a temperature not higher than 40°C, or in good ventilated room under
room temperature,
2. After drying the soil is placed on a polyethylene surface,
3. Manually grind large particles,
4. Take away contaminates (plant residues, stones),
5. Grind the soil and put through a sieve with round holes (diameter: 1-2mm)
6. Store this soil in polyethylene packs or special polyethylene boxes.
Note: Before drying, the soil has to be mixed and make the layer not higher than 1 cm. Sample for analysis
has to be made from not less than 5 random points of this layer of soil
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Extraction methods:
GOST 26204-91 Chiricov method
Extraction solution CH3COOH/liter (0.5M)
Put 30 ml of acetic acid concentrated in half a liter distilled water, mix and fill up to 1 liter with distilled
water.
Procedure
Weigh out 4 g of soil sample.
Add 100 ml of extracting solution.
Mix for 1 hour.
Leave the solution for 18 - 20 hours.
Then shake by hand and filtrate the solution, then the extract is ready for analysis.
GOST 26205-91 Machigin method
Required chemicals: Ammonium Preparation: Dissolve the ammonium carbonate in
carbonate.................. 10.00 g. 500 ml distilled water. Fill up to 1 liter
(NH4)2CO3 with distilled water and mix.
Distilled water
H2O Note: Prepare fresh every other day.
Procedure
Weigh out 5 g of sample.
Add 100 ml of extracting solution.
Shake for 5 minutes.
Leave the solution for 18 - 20 hours at 25 ˚C± 2 ˚C.
Then shake by hand and filtrate the solution, Adjust the pH to ± pH 9, then the extract is ready for analysis.
GOST 26207-91 Kirsanov method
Extraction solution HCl 0.2M/liter
Put 16 ml of hydrochloric acid concentrated (or 20 ml, 32% HCl) in 500 ml distilled water, and bring up to
the 1 liter mark of measure flask with distilled water.
Procedure
Weigh out 10 g of soil sample.
Add 50 ml of extracting solution with a temperature of 18˚C.
Mix for 1 minute.
Leave the solution for 15 minutes.
Then shake by hand and filtrate the solution, then the extract is ready for analysis.
For horizons with peat:
Weigh 1.00 ± 0.01 g of soil instead of 10.
Add 50 ml of extracting solution with a temperature of 18˚C.
Mix for 15 minutes and filtrate the solution, then the extract is ready for analysis.
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REAGENTS
A. Extraction solution Chiricov (1 liter) (rinsing liquid sampler)
Required chemicals: Acetic Acid .................... 30 ml. Preparation: Dissolve the Acetic acid in ± 800 ml
CH3COOH distilled water. Fill up to 1 liter with
Distilled water distilled water and mix.
H2O
Note: Solution is stable for 1 week.
B. Extraction solution Machigin (1 liter) (rinsing liquid sampler)
Required chemicals: Ammonium Preparation: Dissolve the ammonium carbonate in
carbonate.................. 10.00 g. 500 ml distilled water. Fill up to 1 liter
(NH4)2CO3 with distilled water and mix.
Distilled water
H2O Note: Prepare fresh every other day. For
standards and rinsing liquid sampler,
leave the solution for 20 hrs at 25°C and
filter before use.
C. Extraction solution Kirsanov (rinsing liquid sampler)
Rinsing liquid sampler has to be the same as the sample matrix after sample pretreatment according to the
GOST method.
D. Distilled water + Brij 35
Required chemicals: Brij 35 (30%) ................... 1 ml. Preparation: Dilute the Brij 35 in ± 800 ml distilled
Distilled water water. Fill up to 1 liter with distilled water
H2O and mix.
Note: Solution is stable for 1 week.
STANDARDS
Chiricov
Stock solution 1000 mg K2O/liter (1 liter)
Required chemicals: Potassium chloride .. 1.5829 g. Preparation: Dissolve the potassium chloride in ± 800
KCl (dried at 105°C) ml distilled water. Fill up to 1 liter with
Distilled water distilled water and mix.
H2O
Note: Solution is stable for 1 month.
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Working solution
20 mg K2O/liter: Dilute 2.0 ml stock solution 1000 mg K2O/liter to 100 ml with rinsing liquid sampler A.
This standard with GOST 26204-91 Chiricov method represents 500 mg K2O/kg.
16 mg K2O/liter: Dilute 1.6 ml stock solution 1000 mg K2O/liter to 100 ml with rinsing liquid sampler A.
This standard with GOST 26204-91 Chiricov method represents 400 mg K2O/kg.
12 mg K2O/liter: Dilute 1.2 ml stock solution 1000 mg K2O/liter to 100 ml with rinsing liquid sampler A.
This standard with GOST 26204-91 Chiricov method represents 300 mg K2O/kg.
8 mg K2O/liter: Dilute 0.8 ml stock solution 1000 mg K2O/liter to 100 ml with rinsing liquid sampler A.
This standard with GOST 26204-91 Chiricov method represents 200 mg K2O/kg.
4 mg K2O/liter: Dilute 0.4 ml stock solution 1000 mg K2O/liter to 100 ml with rinsing liquid sampler A.
This standard with GOST 26204-91 Chiricov method represents 100 mg K2O/kg.
Machigin
Stock solution 1000 mg K2O/liter (1 liter)
Required chemicals: Potassium chloride .. 1.5829 g. Preparation: Dissolve the potassium chloride in ± 800
KCl (dried at 105°C) ml distilled water. Fill up to 1 liter with
Distilled water distilled water and mix.
H2O
Note: Solution is stable for 1 month.
Working solution
25 mg K2O/liter: Dilute 2.5 ml stock solution 1000 mg K2O/liter to 100 ml with rinsing liquid sampler B.
This standard with GOST 26205-91 Machigin method represents 500 mg K2O/kg.
20 mg K2O/liter: Dilute 2.0 ml stock solution 1000 mg K2O/liter to 100 ml with rinsing liquid sampler B.
This standard with GOST 26205-91 Machigin method represents 400 mg K2O/kg.
15 mg K2O/liter: Dilute 1.5 ml stock solution 1000 mg K2O/liter to 100 ml with rinsing liquid sampler B.
This standard with GOST 26205-91 Machigin method represents 300 mg K2O/kg.
10 mg K2O/liter: Dilute 1.0 ml stock solution 1000 mg K2O/liter to 100 ml with rinsing liquid sampler B.
This standard with GOST 26205-91 Machigin method represents 200 mg K2O/kg.
5 mg K2O/liter: Dilute 0.5 ml stock solution 1000 mg K2O/liter to 100 ml with rinsing liquid sampler B.
This standard with GOST 26205-91 Machigin method represents 100 mg K2O/kg.
Kirsanov
Stock solution 1000 mg K2O/liter (1 liter)
Required chemicals: Potassium chloride .. 1.5829 g. Preparation: Dissolve the potassium chloride in ± 800
KCl (dried at 105°C) ml distilled water. Fill up to 1 liter with
Distilled water distilled water and mix.
H2O
Note: Solution is stable for 1 month.
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Working solution
25 mg K2O/liter: Dilute 2.5 ml stock solution 1000 mg K2O/liter to 100 ml with rinsing liquid sampler C.
This standard with GOST 26207-91 Kirsanov method represents 125 mg K2O/kg.
20 mg K2O/liter: Dilute 2.0 ml stock solution 1000 mg K2O/liter to 100 ml with rinsing liquid sampler C.
This standard with GOST 26207-91 Kirsanov method represents 100 mg K2O/kg.
15 mg K2O/liter: Dilute 1.5 ml stock solution 1000 mg K2O/liter to 100 ml with rinsing liquid sampler C.
This standard with GOST 26207-91 Kirsanov method represents 75 mg K2O/kg.
10 mg K2O/liter: Dilute 1.0 ml stock solution 1000 mg K2O/liter to 100 ml with rinsing liquid sampler C.
This standard with GOST 26207-91 Kirsanov method represents 50 mg K2O/kg.
5 mg K2O/liter: Dilute 0.5 ml stock solution 1000 mg K2O/liter to 100 ml with rinsing liquid sampler C.
This standard with GOST 26207-91 Kirsanov method represents 25 mg K2O/kg.
Note:
1. Prepare the working standards fresh daily.
2. The water used for the reagents and standards must be degassed properly before making up the
reagents and standards. Especially water produced by reverse osmosis or ion exchange equipment
contains a lot of gasses, which must be removed by degassing (degassing procedure see operational
remarks and troubleshooting).
3. For better accuracy in low level analysis, more calibration standards must be added below 20%
standard.
CATALOGUE NUMBERS REQUIRED CHEMICALS
Product Supplier and catnr. Danger classification
Acetic acid (glacial) 100% Merck 100063 flammable, corrosive
Ammonium carbonate Merck 159504 harmful, corrosive
Hydrochloric acid (32%) Merck 100313 corrosive
Brij 35 (30%) Skalar 13900
Potassium chloride Merck 104936
Sodium hydroxide Merck 106498 corrosive
RECOMMENDED OPERATIONAL SETTINGS
1. System sample time: 70 sec., wash time: 70 sec., air time: 0 sec.
2. Module sample time: 30 sec., wash time: 30 sec., air time: 0 sec.
3. Calibration type: 1st order ISO 8466-1.
START UP PROCEDURE FLAMEPHOTOMETER (26710900)
1. Fine: adjust to the maximum (most right) position.
2. Course: adjust to x position from the left.
3. Fuel: first turn to the minimum (most right) position then x turns to the left.
4. Air: switch on air compressor and check pressure at the rear side of the flame photometer.
The pressure must be at least 14 psig or higher.
5. Power: turn on the power of the flame photometer and wait for ignition.
6. Blanc: adjust to approximately 100 on the flame photometer display.
For further details see the flame photometer manual.
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OPERATIONAL REMARKS AND TROUBLESHOOTING
1. The stabilizing time of the system is approximately 10 minutes.
2. Persons using this Skalar method should be familiar with normal laboratory practice. This Skalar
method does not purport to address all of the safety problems, if any, associated with its use. It is the
responsibility of the user to establish appropriate safety and health practices and to ensure compliance
with any national regulatory conditions.
3. The sensitivity of the highest standard 25 mg K2O/liter (Machigin method) ≈ 0.550 AU.
4. The sensitivity of the highest standard 20 mg K2O/liter (Chiricov method) ≈ 0.450 AU.
5. The sensitivity of the highest standard 25 mg K2O/liter (Kirsanov method) ≈ 0.550 AU.
6. The connection between the sampler and the sample pump tube is made of 5175 tube.
7. If the sample take up volume is less than 1.00 ml/min, a bypass is required to increase the sample
stream to at least 1.00 ml/min. For 5210 debubbler, when the sample is 1.00 ml/min and higher use
0.23 ml/min debubble tube.
8. Degassing procedures;
a) Good: degas the water with a helium gas flow of approximately 20 liter/hour with aid of a sparger.
Degas 5 liter water for 15 minutes. This procedure removes all dissolved air or, degas the water by
boiling the water for 10 minutes. Cool down to room temperature before usage.
b) Medium: degas the water with a nitrogen gas flow of approximately 20 liter/hour with aid of sparger.
Degas 5 liter water for 15 minutes. This procedure will remove most of the dissolved air.
c) Bad: degas the water by ultrasonic waves. This procedure will remove a small part of the dissolved air.
MAINTENANCE
1. Daily; When daily analysis is finished rinse all reagent lines with distilled water for 30 minutes.
2. Weekly; To decontaminate the system, rinse 30 minutes with 0.5M sodium hydroxide solution and 30
minutes with distilled water. Rinse the system only if the sampler is turned off. The flame photometer
has to be rinsed separate from the system with distilled water.
3. Monthly: Replace all pump tubing (or shift pump tube one color bridge on pump).
MODULE CONSUMABLES
silicone tube catnr. 3150 sleeves catnr. 5400
polyethylene tube catnr. 3142 sleeves catnr. 5401
polyethylene tube catnr. 5141 pump tube 1.40 ml/min. catnr. 3033
polyethylene tube catnr. 5142 pump tube 2.00 ml/min. catnr. 3035
polyethylene tube catnr. 5145 pump tube 0.42 ml/min. catnr. 3028
U-tube for flame catnr. 90041482
MODULE COMPONENTS
manifold holder catnr. 25200105 inlet connector catnr. 5204
module catnr. 5115 glass coil catnr. 5328
end block catnr. 5109 glass coil catnr. 5329
inlet connector catnr. 5206 debubbler catnr. 5217
inlet connector catnr. 5246 clamps small catnr. 5111 4x
connector catnr. 5201 sinkers catnr. 5380
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REFERENCES
Chemical method (no. 569)
1. GOST 26205-91 Soils. Determination of mobile compounds of phosphorus and potassium by Machigin
method modified by CINAO Extraction with ammonium carbonate solution; Phosphorus: photometric at
710 nm, Potassium: Flame photometry
2. GOST 26204-91 Soils. Determination of mobile compounds of phosphorus and potassium by Chiricov
method modified by CINAO Extraction with Acetic acid solution; Phosphorus: photometric at 710 nm.
3. GOST 26207-91 Soils. Determination of mobile compounds of phosphorus and potassium by Kirsanov
method modified by CINAO Extraction with hydrochloric acid solution; Phosphorus: photometric at 710
nm.
4. Serge, W.M.,”Laboratory automatisation of Flame Photometry in the manufacture of Basic Alkali
Chemicals”, Automation in analytical chemistry, page 123-130.
5. Cappellina, F., Cappelletti, L., “Simultaneous Automated determination of magnesium, sodium and
potassium ions in Potash Salt Industry”, Automation in analytical chemistry, page 295-301.
6. Steele, L.D., Ramsey, K.J., Kane, P.F., “Elimination of aliquoting in automated flame photometric
determination of K2O in fertilisers”, J. Assoc. off. Anal. Chem., Vol. 67, No. 4, 1984, page 847-849.
7. ISO 3696:1987, Water for analytical laboratory use. Specification and test methods.
8. ASTM, D1193, Standard Specification for Reagent Water.
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