PS5469-2020 Liquid Nutrient Supplement

PS: 5469-2020
PAKISTAN STANDARD SPECIFICATION FOR
LIQUID NUTRIENT SUPPLEMENT
(ALL RIGHTS RESERVED)

PAKISTAN STANDARDS AND QUALITY CONTROL AUTHORITY
STANDARDS DEVELOPMENT CENTRE, STANDARDIZATION WING
1ST FLOOR, ST-7-A, BLOCK-3, GULISTAN-E-JOHER, Karachi
Licensed to Company M/s Avan Agro

Order No. PSQCA/SDC/AA/22-1
Single user license only. copying and networking prohibited
PS: 5469-2020
PAKISTAN STANDARDS SPECIFICATION

FOR
LIQUID NUTRIENT SUPPLEMENT
0. FOREWORD
0.1 This Pakistan Standard was adopted by Pakistan Standards & Quality Control Authority on
19 August 2020 after the draft finalized by the Fertilizers and Allied Product Technical Committee had
been approved by the National Standards Committee for Chemical Division.
0.2 The use of liquid Nutrient supplement is increasing globally to supplement the crop needs for balanced
fertilization in intensified agriculture system. Liquid or fluid Nutrient supplement are best suited for
fertigation, variable rate application required for different crops at different plant stages, wide variety of
fertilizer placement and best adapted split applications. High nutrient use efficiency, homogeneous blends,
handling convenience and environmental benefits give fluids a distinct economic appeal.
0.3 The Sectional Committee responsible for the preparation of this draft felt that it is necessary to lay down
specifications on liquid Nutrient supplement to safeguard the interests of farming community and to
protect them from using wrong types or grades of liquid Nutrient supplement as well as to safeguard the
interest of the manufacturers.
0.4 While preparing this standard the views of the producers, consumers and testing authorities were taken into
consideration by the Sectional Committee. Due weightage to the standards prevailing in different countries
of the world was also given.
0.5 For the purpose of deciding whether the particular requirements of this standards complied with, the final
value observed or calculated, expressing the result of a test or analysis shall be rounded off in accordance
with or calculated expressing the result of a test or analysis, shall be rounded off in accordance with PS:
103 : 1960 “Rules for Rounding Off Numerical Values”. The number of places retained in the rounded off
value should be the same as those of the specified value in this standard.
0.6 This standard is intended mainly to cover the technical provisions relating to the supply of the material,
and it does not cover all the necessary provision of a contract.
1. SCOPE
1.1 This standard provides requirement and methods of test for high analysis liquid Nutrient supplement.
2. TERMINOLOGY
2.1 For the purpose of this standard, following definitions, in addition to definitions given in PS: 582:1966
“Glossary of Terms used in Fertilizer Industry”, shall apply.
2.1.1 Liquid Nutrient supplement: are fluid supplement, applied in soil and/or as foliar application to provide
nutrients to plant, and include the following types:
1. Solution
2. Suspension
2.1.2 Solution: clear mixture in which all nutrients are fully dissolved.
2.1.3 Suspension: saturated nutrient mixture produced by mixing solid fertilizer with water followed by adding
emulsifier to maintain suspension, reduce settling and facilitate even distribution of nutrients at application.
Chemical Division P-1/38

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2.1.4 Fertilizer Grade Analysis: minimum guaranteed percentage (w/v) of nutrient content in liquid Nutrient
supplement fertilizers in terms of Nitrogen (N), available phosphorus pentoxide (P2O5), water soluble potassium
oxide (K2O), Calcium (Ca), Magnesium (Mg), Sulfur (S), Zinc (Zn), Iron (Fe), Manganese (Mn), Copper (Cu),
Boron (B) and other trace elements, as mentioned on the packing.
2.1.5 Available Phosphate: plant available phosphate soluble in neutral ammonium citrate solution (i.e. Total P2O5 -
Citrate Insoluble P2O5).
3. REQUIREMNETS
3.1 The product shall contain nutrients according to the requirements specified in Table 1.
Table 1. Requirement for Fertilizer Grade Analysis of Liquid Nutrient supplement.
Contents
Category Sub-Category Nutrients Method
(w/v)
A Single Nutrient A1 Macro Nutrients Total N Min 20% Appendix B
Available P2O5 water
Min 20% Appendix C
soluble
Soluble K2O Min 30% Appendix D
A2 Secondary Nutrients Ca, Mg Min 10% Appendix E
-- Min 50% Appendix F
A3 Micro Nutrients Zn, Fe, Mn, Cu Min 10% Appendix E
B Min 5% Appendix E
B Multi Nutrient B1 Macro Nutrients N, P2O5, K2O Appendix B,
Min 20%
(Combination of any two C, D
or more nutrients) B2 Secondary Nutrients Ca, Mg, S as Sulphate Appendix E
Min 10%
SO4 and F
B3 Micro Nutrients Zn, Fe, Mn, Cu,B Min 10% Appendix E
B4 Macro + Secondary N, P2O5, K2O, Ca, Mg, Appendix B,
Min 20%
Nutrients S C, D, E, F
B5 Macro + Micro N, P2O5, K2O, Zn, Fe, Appendix B,
Min 20%
Nutrients Mn,Cu, B C, D, E
B6 Secondary + Micro Ca, Mg, S, Zn, Fe,
Min 20% Appendix E, F
Nutrients Mn, Cu, B
B7 Macro + Secondary + N, P2O5, K2O, Ca,
Appendix B,
Micro Nutrients Mg, S, Zn, Fe, Mn, Cu, Min 20%
B
C, D, E, F
C Chelated Nutrients
Appendix E-
(Any one or combination of Micro Nutrients Zn, Fe, Mn, Cu Min 5%
2.3
two or more nutrients)
Liquid or Suspension, Visual
D Physical appearance
emulsion inspection
E Insoluble contents Max 1% Appendix G
F Biurate, in case of N Max 1% Appendix B-5
G Sodium (in case of K, secondary, micro and multi-nutrients) Max 1% PS 1501
H Chloride (in case of N, P and K) Max 1% PS 1501
I Tolerance Nutrients On lower side Max 5%
Impurities On higher side Max 5%
4. PACKING AND MARKING:

4.1 Packing. The material shall be packed and supplied in sound, strong, leakage proof packages or
container as agreed to between producer/marketer/distributor and purchaser/vendor.
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4.2 Marking. The container shall be securely closed and marked with following information:
a. Name of material : Product Name
b. Contents : fertilizer grade analysis of each nutrient in %w/v
c. Name and address of the manufacturer/importer/distributor; trade mark if any
d. Volume minimum in 1 litre.
e. Nitrogen source (in case of liquid fertilizer products containing N): Organic, Ammonium and/or Nitrate
f. Only for Agriculture use and keep out of reach of Children’s.
4.3 Store in cool, clean, dry and well-ventilated area at room temperature away from oxidizers, acids, and food and
drinkable items.
5.0 SAMPLING:
5.1 The representative samples of the material shall be drawn as described in Appendix “A”.
APPENDIX ‘A’
SAMPLING OF LIQUID FERTILIZERS FROM CONTAINERS AND

PREPARATION OF THE SAMPLE FOR ANALYSIS
A-1 SCOPE:
The method is applicable to the sample of liquid fertilizer materials from containers.
A-2 SAMPLING:
Liquid fertilizer samples are taken, after mixing thoroughly, from randomly selected containers, in accordance
with prescribed sampling rates.
A-3 SCALE OF SAMPLING:
A-3.1 Lot - All the containers in a single or many consignments of the product from a single batch of manufacture
shall constitute the lot. If a consignment is consisted of different batches of manufacture, each batch shall be
considered a lot.
A-3.2 Composite Sample—Due to specific nature of liquid fertilizers, composite sample is not possible, therefore,
three full container of liquid fertilizer shall taken as Test Sample at random from each lot.
A-4 PROCEDURE
A-4.1 Test Samples from Containers – Randomly select three full containers for each lot.
A-4.2 Test Sample - Labeled each test sample with all particulars of sampling. One test sample shall be sent to testing
laboratory for fertilizer grade analysis. Second test sample, be kept at secure place agreed between purchaser,
vendor and respective authority.
A-4.3 Referee Sample - The third sample bearing the seals and signatures of purchaser/vendor and sampling authrotiy,
shall constitute the referee sample, to be used in case of dispute between purchaser/vendor and regulatory
autohrity, and it shall be kept with purchaser/vendor.
A-5 NUMBER OF TESTS:
A-5.1 Test for the determination of nutrients given on the label shall be conducted on each of the individual test
sample.
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APPENDIX ‘ B ’
TOTAL NITROGEN
B-0 Total nitrogen in a sample of mixed or complex fertilizer may include amide, ammoniacal and nitrate forms of
nitrogen as well as some nitrogen in the organic matter present in mixed fertilizer.
This section includes the following four procedures for nitrogen estimation:-
B-1 Total nitrogen in nitrate free fertilizers.
B-2 Total nitrogen in fertilizers having nitrates.
B-3 Total ammoniacal nitrogen in fertilizers.
B-4 Total nitrogen in fertilizers having only nitrates a nitrate and ammoniacal nitrogen.
B-5 Biuret content of mixed fertilizers.
Procedures B-3 and B-4 may be used to determine the percentage of nitrate and ammoniacal nitrogen. A
qualitative procedure for detection of nitrates is also included in this section.
B-0.1 Detection of Nitrates:
Mix 5 ml sample with 25 ml distilled H2O, and filter. To 1 volume of this solution add 2 volumes, H2SO4 free
form HNO3 and oxides of N, and let it cool. Add few drops concentrated FeSO4 solution in such a manner that
fluids do not mix. If nitrates are present junction shows at first purple, afterwards brown, or if only minute
quantity is present, reddish color. To another portion of solution add 1 ml 1% NaNO3 solution and test as
before to determine whether enough H2SO4 was added in first test.
B-1 IMPROVED KJELDAHL METHOD FOR NITROGEN CONTENT OF

NITRATE-FREE FERTILIZERS
B-1.1 SCOPE:
This procedure is applicable to the analysis of nitrate-free fertilizers.
B-1.2 Summary:
Nitrogen in the sample is converted to ammonium sulfate by means of the kjeldahl method. Caustic soda is
added and the liberated ammonia is distilled into a boric acid solution. The ammonia is titrated with a standard
hydrochloric acid solution and the nitrogen content calculated from the data. Nitrogen content is reported in
weight percent to the nearest 0.1%.
B-1.3 Apparatus:
(1) Kjeldahl Flask—500-800 m1. Capacity flask of hard moderately thick, well annealed glass.
(2) Digestion Unit—consisting of heater (gas or electric) a refractory support for the flask and a bracket to
hold the neck of the flask titled at an angle from the vertical. The heater should be capable of
adjustment such that it can bring 250 m1. Of water in a kjeldahl flask from 25ºC to a rolling boil in five
minutes.
(3) Distillation Unit—Use 500-800 m1. Kjeldahl or other suitable flask, with rubber stopper through which
passes lower and of efficient scrubber bulb or trap to prevent mechanical carry-over of NaOH during
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distillation. Connect upper end of bulb tube to condenser tube by rubber tubing. Trap outlet of
condenser in such way as to ensure complete absorption of NH3 distilled over into acid in receiver.
B-1.4 Reagents:
Unless otherwise indicated, the purity of all regents is intended to be of reagent grade.
(1) Mercury (or mercuric oxide, HgO)
(2) Potassium Sulfate, Powdered—(or anhydrous sodium sulfate)
(3) Sulfuric Acid—93 to 98% H2SO4, nitrogen free.
(4) Sulfide Solution (or thiosulfate solution).—Dissolve 40 grams of potassium sulfide or sodium sulfide in
1 liter of water (or dissolve 80 g. of sodium thiosulfate Na2S2O3.5H2O in 1liter of water).
(5) Zinc.—Granular, 20-mesh.
(6) Sodium Hydroxide Solution—Dissolve 450 g of solid, nitrate-free sodium hydroxide in water, cool
and finally dilute to 1 liter. The specific gravity of the solution should be 1.36 or higher in order to
ensure that it will remain in a lower layer when add without agitation to the diluted sulfuric acid
digestion mixture.
(7) Boric Acid Solution—Dissolve 50 g of boric acid, H3BO3, in one liter of boiling water.
(8) Methyl Purple Indicator Solution—Available from most chemical supply companies in solution form.
(9) Standard Hydrochloric Acid Solution, N/10.—Dilute 8.4 ml of reagent grade hydrochloric acid (36.5—
38%) to one liter with water and mix well. Standardize the solution against dried, primary standard
grade sodium carbonate using methyl purple as the indicator.
B-1.5 Sampling: If the volume of sample as received at the laboratory is greater than 500ml, reduce the gross sample
to between 250 ml Store in tightly stoppers bottles.
B-1.6 Procedure:
Reference to water in the following paragraphs mean distilled or deionized water:-
1. Take out 0.5 to 2.2 ml of the sample. The optimum sample volume is one which will require a 40 to 50
ml titration in step (14).
2. Transfer the weighed sample to a kjeldahl flask. Avoid contacting the sides of the flask neck with the
sample.
3. Add 0.65 g. of mercury (or 0.7 g. of mercuric oxide), 15 g. of powdered potassium sulfate (or 15 g. of
anhydrous sodium sulfate) and ml of sulfuric acid (93-98%) to the flask. If a sample weight greater than
2.2 g. was used, the volume of sulfuric acid introduced should equal 10 ml for each gram of sample.
4. Run a blank determination along with each batch of samples. Add to another digestion flask the same
quantities of mercury (or mercuric oxide), potassium sulfate (or sodium sulfate) and sulfuric acid that
were added to the sample flask. Carry the blank through the following steps in exactly the same manner
as the sample(s).
5. Place the flask on the heater and support the neck in a inclined position. Heat the flask gently until
frothing ceases. A small amount of Paraffin may be added to reduce frothing.
6. Increase the heat and boil the solution briskly until it clears. Continue the boiling for 30 minutes after
the solution has cleared (2 hours for samples containing organic matter).
7. Cool the solution and carefully add, with continuous swirling, 200 ml of water. Cool the solution to
25ºC., or lower.
8. Add 25 ml of the sulfide solution (or thiosulfate solution) and swirl the flask to mix the contents and
precipitate the mercury.
9. Measure 25 ml of boric acid solution into a 300-ml Erlenmeyer flask means of a graduated cylinder and
add 5 drops of methyl purple indicator solution.
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10. Place the Erlenmeyer flask beneath the condenser of the distillation assembly so that the delivery tip is
located below the surface of the acid solution. Tilt the flask to provide a grater depth of boric acid
solution and make sure that the delivery tip extends as far as possible into the solution without actually
touching the bottom of the flask. Attach the connecting tube and spray trap to the upper end of the
condenser.
11. Add a few granules of zinc to the kjeldahl flask to prevent bumping, title the flask and carefully add 55
ml of sodium hydroxide solution (450 g./1). Do not agitate the flask during the addition. The amount of
sodium hydroxide added should be enough to make the solution strongly alkaline, when the solution is
mixed in the following step.
12. Immediately connect the digestion flask to the spray trap. Swirl the flask to mix the contents
thoroughly. Apply heat to the flask so as to bring the contents t a boil rapidly. Continue the heating
until at least 150 ml of distillate has been collected in the receiver.
13. Lower the receiver flask so that the deliver tip is above the surface of the solution and turn off the heat.
Several minutes after turning of the heat, wash of the delivery tip of the condenser into the receiver
with distilled water.
14. Titrate the solution in the receiving flask with the standard acid solution to the purple end point. The
green color of the indicator fades into gray near the end point, and the end point is reached when the
gray just disappears and only purple color remains. Record the volume of standard acid required to
titrate the absorber solution.
B-1.7 Calculation:
Calculate the nitrogen content by means of the following equation:
C = (A-B)×N×0.01401×100
V
Where
A is the volume of standard acid required to titrate the sample, in ml
B is the volume of standard acid required to titrate the blank, in ml
N is the normality of the Standard acid.
V is the volume of the sample, in ml
C is the concentration of nitrogen in the sample, in % (vol.)
B-1.8 Reporting:
Report the results as
Nitrogen___________% (vol.)
B-2 IMPROVED KJELDAHL METHOD FOR NITROGEN CONTENT OF FERTILIZERS CONTAINING

NITRATES
B-2.1 Scope:
This method is intended for the determination of nitrogen in fertilizers containing nitrates.
B-2.2 Summary:
Nitrogen in the sample is converted to ammonium sulfate by means of the kjeldahl method. Conversion to
ammonia of nitrogen present as nitrate is made possible by the inclusion of salicylic acid and sodium thiosulfate
in the digestion mixture. Caustic soda is added and the liberated ammonia is distilled into a boric solution. The
ammonia is titrated with a standard hydrochloric acid solution and the nitrogen content calculated from the
data. Nitrogen concentration is reported in weight per cent to the nearest 0.1%
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B-2.3 Apparatus:
(1) Kjeldahl Flask—800-ml capacity flask of hard moderately thick, well annealed glass.
(2) Distillation Unit—Consisting of a heater, a connecting tube fitted with a spray trap, and a condenser.
B-2.4 Reagents:
Unless otherwise indicated, the purity of all reagents is intended to be of reagent-grade.

(1) Sulfuric Acid—93-98% H2SO4 nitrogen-free.
(2) Salicylic Acid—nitrogen-free
(3) Sodium Thiosulfate—crystals, Na2S2O3.5H2O. Zinc powder (dust) may be used in place of sodium
thiosulfate, if desired.
(4) Mercury. (or mercuric oxide, Hg O.)
(5) Potassium Sulfate—powdered (or anhydrous sodium sulfate).
(6) Sulfide Solution.(or thiosulfate solution).—Dissolve 40 g. of potassium sulfide or sodium sulfide in 1
liter of water (or dissolve 80 g. of sodium thiosulfate, Na2S2O3.5H2O in 1 liter of water).
(7) Zinc—Granular, 20-mesh.
(8) Sodium Hydroxide Solution—Dissolve 450 g. of solid, nitrate-free sodium hydroxide in water, cool
and finally dilute to 1 liter. The specific gravity of the solution should be 1.36, or higher in order to
ensure that it will remain in a lower layer when added to the diluted sulfuric acid digestion mixture.
(9) Boric Acid Solution—Dissolve 50 g. of boric acid, H3BO3, in one liter of boiling water.
(10) Methyl Purple Indicator Solution—Available from most chemical supply companies in solution
form.
(11) Standard Hydrochloric Acid Solution, N/10—Dilute 8.4 ml of reagent hydrochloric acid (36.5—
B-2.5 Sampling:
Reduce the gross sample to a quantity sufficient of analysis and store in tightly stoppered bottles.
B-2.6 Procedure:
References to water in the following paragraphs mean distilled or deionized water:-

(1) Take out 0.5 to 2.2 ml of the sample. The optimum sample volume is one which will require a 40- to
50- ml titration in step (16).
(2) Transfer the weighed sample to a kjeldahl flask, Avoid contacting the sides of the flask neck with the
sample.
(3) Add 40 ml of sulfuric acid (93-98% Na2S2O3.5H2O). If desired, 2 g. of zinc dust (net granulated zinc
or fillings) may be added in place of the sodium thiosulfate. Shake and let stand for five minutes.
(4) Add 5 g. sodium thiosulfate crystals (Na2S2O3.5H2O). If desired, 2 g. of zinc dust (net granulated zinc
or fillings) may be added in place of the sodium thiosulfate. Shake and let stand for five minutes.
(5) Warm the flask over low heat until frothing ceases. Remove from the heat.
(6) Add 0.65 g. of mercury (0r 0.7 g. of mercuric oxide) and 15 g. of powdered potassium sulfate (or 15 g.
or anhydrous sodium sulfate).

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(7) Run a blank determination along with each batch of samples. Add to another digestion flask the same
quantities of reagents that were added to the samples flask. Carry the blank through the following steps
in exactly the same manner as the samples(s).
(8) Boil the solution until it clears. Continue the boiling for 30 minutes after the solution has cleared (2
hours for samples containing organic matter).
(9) Cool the solution and carefully add, with continues swirling 200 ml of water. Cool the solution to 25ºC
or lower.
(10) Add 25 ml of the sulfide solution (or thiosulfate solution) and swirl the flask to mix the contents and
precipitate the mercury.
(11) Measure 25 ml of boric acid solution into a 300-ml Erlenmeyer flask by means of a graduated
cylinder and add drops of methyl purple indicator solution.
(12) Place the Erlenmeyer flask beneath the condenser of the distillation assembly so that the delivery tip is
located below the surface of the acid solution. Tilt the flask to provide a greater depth of boric acid
condenser.
(13) Add a few granules of zinc to the kjeldahl flask to prevent bumping tilt the flask and carefully add 55
ml of sodium hydroxide solution (450 g./1). Do not agitate the flask during the addition. The amount of
(14) Immediately connect the digestion flask to the sprat trap. Swirl the flask to mix the contents thoroughly.
Apply heat to the flask so as to bring the contents to boil rapidly. Continue the heating until at least 150
ml of distillate has been collected in the receiver.
(15) Lower the receiving flask so that the delivery tip is above the surface of the solution and turn off the
heat. Several minutes after turning off the heat, wash off the delivery tip of the condenser into the
receiver with distilled water.
(16) Titrate the solution in the receiving flask with the standard acid solution to the purple end point. The
green color of the indicator fades into gray near the end point, and the end point is reached when the
gray just disappears and only purple color remains. Record the volume of standard acid required to
B-2.7 Calculation:
% Nitrogen = (A-B)×N×0.01401×100
V
Where
B is the volume of standard acid required to titrate the sample, in ml
N is the normality of the standard acid
B-2.8 Reporting:
Report the result as
Nitrogen----------------------% (vol.)

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B-3 AMMONICAL NITROGEN IN LIQUID FERTILIZERS
B-3.1 Scope:
The procedure is applicable to the determination of nitrogen present or available in liquid fertilizers as ammonia
or ammonium ion. It is not applicable to samples containing urea. Magnesium ammonium phosphate
(MgNH4PO4), or ferrous ammonium phosphate (FeNH4PO4).
B-3.1 Summary of Method:

A weighed amount of the sample is steam distilled in the presence of magnesium oxide. Ammonia present as
free ammonia or ammonium is driven over into a boric acid solution and the absorbed ammonia is titrated with
standard acid. Results are reported as percent ammoniacal nitrogen to the nearest 0.1%.
B-3.3 Apparatus
(3) Kjeldahl Flask—800-ml capacity flask of hard moderately thick, well annealed glass.
(4) Distillation Unit—Consisting of a heater, a connecting tube fitted with a spray trap, and a condenser.
B-3.4 Reagents:
(1) Magnesium Oxide (carbonate free)

(2) Standard Hydrochloric Acid Solution. N/10.—Dilute 8.4 ml of regent grade hydrochloric acid (36.5—
(3) Boric Acid Solution—Dissolve 50 g. of boric acid H3 BO3, in one liter of boiling water.
(4) Methyl Purple Indicator Solution—available from most chemical supply companies in solution form.
B-3.5 Procedure:
(1) Take out 0.7 to 3.5 ml of the sample. The optimum sample volume is one which will require a 40 to 50-
ml titration. Transfer the sample to the kjeldahl flask and add about 300 ml of distilled water.
(2) Measure 25 ml of boric acid solution into a 300 ml Erlenmeyer flask by means of a graduated cylinder
and add 5 drops of methyl purple indicator solution.
(3) Add 2 g. or more of the carbonate-free magnesium oxide to the kjeldahl flask. Connect immediately to
the other end of the condenser tube. Mix the contents by shaking.
(4) Apply heat to the flask so as to bring the contents to a rapid boil. Continue the heating until at least 150
ml of distillate has been collected in the receiver.
(5) Lower the receiving flask so that the delivery tip is above the surface of the solution and turn off the
heat. When cool wash off the delivery tip of the condenser into the receiver with distilled water.
(6) Run a blank with each batch of samples. Add 300 ml of distilled water and 2 g. of magnesium oxide to
a kjeldahl flask and follow the same steps that are used with the sample.
green color of the indicator fades to a gray near the end point and the end point is reached when the
gray disappears and only the purple color remains. Record the volume of the standard acid required to

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B-3.6 Calculations:
Calculate the ammoniacal nitrogen content by the equation
% Ammoniacal Nitrogen = (A-B)×N×0.0141×100

V
Where
B is the volume of acid required to titrate the blank, in ml
B-2.8 Reporting:
Report the results to the nearest 0.1 % as
Ammoniacal Nitrogen----------------------% (Vol.)
B-4.4 AMMONIUM AND NITRATE NITROGEN BY DEVARD’S METHOD
B-4.1 Scope:
This procedure is applicable to the analysis of fertilizers containing only the two inorganic forms of
ammoniacal and nitrate nitrogen. It is not applicable in the presence of organic matter, calcium cynamide and
urea.
B-4.2 Summary :
Nitrate is reduced to ammonium by nascent hydrogen produced by the action of NaOH upon Zn and A1
(components of Devarda’s alloy) and the total ammonium is volatilized as NH3 into boric acid as in the total
nitrogen procedure. The ammonia is titrated with a standard hydrochloric acid solution and the nitrogen content
calculated in weight percent to the nearest 0.1%.
B-4.3 Apparatus:
Kjeldahal flask: 800 ml capacity flask of hard moderately thick well annealed glass.
Distillation Unit:
Use 800 ml kjeldahl or other suitable flask, fitted with rubber stopper through which passes lower end of an
efficient scrubber bulb or trap to prevent mechanical carryover of NaOH during distillation. Connect upper end
of bulb tube by rubber tubing. Trap outlet of condenser in such a way as to ensure complete absorption of NH3
distilled over into acid in a receiver.
B-4.4 Reagents:
(1) Devarda’s Alloy—Prepare this reagent by ball milling a good quality alloy until the product will pass a
100 mesh screen and at least 75 percent it will pass a 300 mesh screen. Store the finely divided alloy in
a tightly stoppered bottle.
Sodium Hydroxide Solution—Dissolve 450 g of solid nitrate free sodium hydroxide in water, cool
and finally dilute to 1 liter. The specific gravity of the solution should be 1.36, or higher, in order to
ensure that it will remain in a lower layer when added to the distillation flask.
(2) Boric Acid Solution—Dissolve 50 g. of Boric acid, H3 BO3 in one liter of boiling water.
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(3) Methyl Purple Indicator Solution—Available from most chemical companies in solution form.
(4) Standard Hydrochloric Acid Solution. N/10—Dilute 8.5 ml of reagent grade hydrochloric acid
(36.5—38 %) to one liter with water and mix well. Standardize the solution against dried, primary
standard grade sodium carbonate using methyl purple as the indicator.
B-4.5 Procedure
Reference to water in the following paragraphs mean distilled or deionized water.

(1) Take out 0.35 to 0.5 ml of the sample. The optimum sample weight is one which will require a 40 to 50
ml titration in step 8.
(2) Transfer the weighed sample to 800 ml Kjeldahl flask. Avoid contacting the sides of the flask neck with
sample. Add 300 ml of water.
(3) Measure 25 ml of boric acid solution into a 300 ml Urlenmeyer flask by means of a graduated cylinder
and add 5 drops of methyl purple indicator solution.
(4) Place the Urlenmeyer flask beneath the condenser of the distillation assembly so that the delivery tip is
located below the surface of the acid solution. Tilt the flask to provide greater depth of the boric acid
condenser.
(5) Add 3 g. fo Devard’s alloy and add 55. Ml of sodium hydroxide solution (450 g/1) to the kjeldahl flask
containing the fertilizer material and water. Do not agitate the flask during the addition. The amount of
(6) Immediately connect the digestion flask to the spray trap. Swirl the flask to mix the contents
thoroughly. Apply heat to the flask so as to bring the contents to boil rapidly. Continue the heating until
at least 300 ml or more of distillate has been collected in the receiver. It is necessary to carry the
distillation nearly to dryness to obtain complete reduction of all nitrate.
(7) Run a blank determination along with each batch of samples. Add to another digestion flask the same
quantities of reagents that were added to the sample flask. Carry the blank through all the steps in
exactly the same manner as the sample(s).
green colour of the indicator fades to a grey near the end point and the end point is reached when the
grey disappears and only the purple colour remains. Record the volume of the standard acid required to
B-4.6 Calculations
Calculate the nitrogen content (Ammoniacal+Nitrate) of the sample by equation:
% N = (A-B)×N×0.0141×100
V
Where
B is the volume of acid required to titrate the blank, in ml

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B-2.8 Reporting:
Report the results to the nearest 0.1 % as total N (Ammoniacal+Nitrate nitrogen).
B-5 BIURET CONTENT OF MIXED FERTILIZERS

COLORIMETRIC METHOD
B-5.1 Scope:
The method is intended for the determination of the biuret content of mixed fertilizers.
B-5.2 Summary of Method:

A known weight of sample is stirred in a C02—free distilled water to dissolve the biuret and the solution is
filtered. The filtrate is passed through an ion exchange column to remove interference such as ammonium ions.
The eluate is then treated with copper sulfate in the presence of alkaline tartrate solution; the biuret in the
sample reacts to form a copper complex, the intensity of which is proportional to the biuret content. The color
intensity is measured at 550 mu and with the absorbance known, the percent biuret is determined from the
calibration curve. Results are reported to the nearest 0.01 weight percent.
B-5.3 Apparatus:
(1) Spectrophotometer—Capable of measuring absorbance at 555 mu, such as the Beckman instrument.
Photoelectric colorimeters fitted with a 500—570 millimicron (or 520—580 millimicron) filter are
acceptable.
(2) Absorption Cells—Hatched pair 50 mm. light path length.
(3) Water Baths—Capable of maintaining temperatures of 30±5ºC and 50±5ºC.
(4) Filter Paper—Whatman 1 or its equivalent.
B-5.4 Reagents:
Unless otherwise indicated, the purity of the following materials should be of reagent grade:-
(1) CO2 Free Distilled Water—Prepare by boiling distilled water. Cool prepare fresh daily.
(2) Alkaline Tartrate Solution—Dissolve 40 g. of sodium hydroxide in 500 ml of water, stopper the
container and allow to cool, add 50 g. of sodium potassium tartrate (NaKC4H406.4H20), and agitate
the solution to dissolve the crystals. Dilute to 1 liter and mix well. Allow the solution to stand one day
before use.
(3) Copper Sulfate Solution—Dissolve 15 g of copper sulfate (CuSO45H20), in CO2—free distilled water
and dilute to 1 liter.
(4) Biuret Standard Solution—Dissolve 1 mg./ml Dissolve 250±1 mg. of biuret in CO2—free distilled
water and dilute to the mark in a 250 ml volumetric flask.
(5) Methyl Red Indicator—Dissolve 1 g. of methyl red in 200 ml of ethyl alcohol.
(6) Sulfuric Acid, 0.1N—Add 2.8 ml of concentrated sulfuric acid to approximately 500 ml of water in a 1-
liter volumetric flask and fill to the mark with additional water. Mix well. Standardization of the
solution is not required.
(7) Ion Exchange Resin—Fill a 50 ml Biuret with 30 cm column of Amberlite IR 120 (H) resin on a glass
wool plug. (Regenerate the column after each use by passing 100 ml of H2SO4 (1: 9) or HCI (1 : 4)
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through the column at 5 ml/min. then wash with water until the PH of the effluent is greater than 6.
The Amberlin IR 120 (H) resin is available from Rohm and Haas, Philadephia, Pennsylvania, or a
comparable ion exchange resin may be used.
B-5.5 Calibration:
(1) Pipet separately 2, 10,20,30,40, and 50ml of the biuret standard solution regant (4) in 100 ml
volumetric flasks. These will contain 2, 10, 20, 30, 40 and 50 mg. biuret, respectively.
(2) Adjust the volume in each flask to about 50 ml with CO2—free distilled water.
(3) Add one drop of methyl red into each flask and neutralize with 1 or 2 drops of 0.1N sulfuric acid to a
pink color and swirl.
(4) While swirling, pipet into each flask 20 ml of alkaline tartrate solution, Reagent (2), followed by 20 ml
of copper sulfate solution, Reagent (3).
(5) Fill each flask to the mark with CO2—free distilled water and shake for 10 second.
(6) Allow the flasks to stand for 15 minutes at 30±5ºC. If the room temperature is not 30±5ºC, place the
flasks in a water bath maintained at 30±5ºC.
(7) Prepare a reagent blank, using the same quantities of reagents and conditions but excluding the biuret
standard solution.
(8) Fill one of the absorption cells with the regent blank and plight path in the spectrophotometer. Set the
wavelength at 555 millimicrons. Adjust the absorbance to zero in accordance with instructions for the
particular instrument.
(9) Fill the same cell with one of the calibration standards and determine the absorbance at 555
millimicrons. Record the absorbance reading.
(10) Repeat the absorbance measurement for each of the remaining calibration standards. All measurement
should be conducted so that no standard is allowed to stand for more than 30 minutes measured from
the time it was placed in the 30ºC bath.
(11) Prepare a calibration curve on rectilinear paper by plotting the absorbance values against the
corresponding weights of biuret in the standards in mg.
B-5.6 Procedure:
(1) Take 10 ml of the sample under test into a 150 ml beaker. Dissolve in 50 ml of the CO2—free distilled
preheated at 50±5ºC.
(2) Stir the solution for 30 minutes and maintain the temperature at 50±5ºC by using a water bath capable
of maintaining a temperature of 50±5ºC.
(3) Filter the solution into a 100 ml volumetric flask using a medium sized filter paper. Rinse the beaker
and the stirrer with small portions of CO2—free distilled water and add the rinsings to the filter. Fill the
flask to the mark with CO2—free distilled water.
(4) Transfer 25 ml aliquot of the filtrate into the ion exchange column; adjust the flow to 4—5 ml/minute,
collect the eluate in a 100 ml volumetric flask.
(5) When the liquid level reaches the top of the resin bed, wash with two ml portions of CO2—free
distilled water, and add the washings to the eluate in the flasks.
(6) Add 1 or 2 drops of methyl red indicator and IN NaOH to a yellow color. Add a few drops of 0.IN
N2SI4 until the solution just turns pin. Fill the flask to the mark CO2—free distilled water, shake and
mix thoroughly.
(7) Piet 50 ml of the solution into a 100 ml volumetric flask and proceed as in CALIBRATION, steps (3)
through (8).
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(8) Fill the sample cell with the sample under test and determine the absorbance at 555 m/micron.
(9) From the calibration curve, determine the mg. of biuret that corresponds with the absorbance reading.
B-5.7 Calculation:
Calculate the percent of biuret in the sample by the following equation:-
B = V × 100__________
V1 × 1000 × 25 × 50
100 100
Simplifying:
B = V1 __________
V × 1.25
Where:
V is the volume of the sample in ml
V1 is the biuret content of the sample as read from the calibration curve in mg.
B is the vol. percent biuret in the sample. The constant 25 and 50 are Aliquot portions.
100 100
B-5.8 Reporting:
Report the result to the nearest 0.01 % as :
Biuert Content _____________% (vol.)
APPENDIX ‘C‘
C.0 PHOSPHORUS CONTENT OF FERTILIZERS:
Available Phosphorus in liquid fertilizers refers to the plant available phosphorus which includes both water
soluble and citrate soluble forms.
This section includes the following test procedures:-

C1—Total Phosphorus content of fertilizers
C2—Water soluble Phosphorus content of fertilizers
C3—Citrate insoluble Phosphorus content of the fertilizers.
Test procedures C1 and C3 may be used to determine citrate soluble (Total Phosphorus 3/M citrate insoluble
phosphorus) phosphorus content of the fertilizers.
C-1 PHOSPHORUS (TOTAL CONTENT OF FERTILIZERS)
C-1.1 Scope:
The procedure is applicable to phosphorus-containing fertilizers such as the superposphates, mixed fertilizers,
nitrophos and ammophos complexes and fertilizer raw materials. The sepctrophotometric alternative is not
applicable to materials yielding colored solutions or solutions containing ions other than orthophosphate which

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from colored complexes with molybdovanadate and is not recommended for basic slag. The volumetric method
may be used in all cases.
C-1.2 Summary of Method:-

The sample is dissolved in acid and the phosphorus content of the solution determined by either a volumetric or
spectrophotometric method. The volumetric option involves precipitation of the phosphate with molybdate
solution, removal of the precipitate by filtration, dissolution of the precipitate in an excess of standard alkali
solution and titration of the excess alkali with standard acid. In the spectrophotometric alternative the sample
solution is reacted with molybdovanadate reagent and the absorbance of the resulting product measured in a
spectrophotometric and the phosphorus content is reported as percent P205 to the nearest 0.01%.
C-1.3 Apparatus:
(1) Agitator—A machine capable of shaking Erlenmeyer flasks such as a wrist-type shaker or any device
capable of stirring the contents of a beaker, such as magnetic stirrer, may be used.
(2) Sintered Crucibles—Porcelain, 30 ml capacity, fine retain fine precipitates may be used.
C-1.4 Reagents:
Reference to water in this and the following sections shall be understood to mean distilled water, or water of
equivalent purity:
(1) Molybdate Solutions—Dissolve 100 g. of molydbic anhydried (Mo03) in a mixture of 144 ml of
concentrated ammonium hydroxide and 271 ml of water. Cool and pour the solution slowly, with
constant stirring into a cool mixture of 489 ml of concentrated nitric acid and 1148 ml of water. Keep
the final mixture in a warm place for several days until a portion heated to 40ºC deposit no yellow
precipitate. Decant the solution from any sediment and store in glass stoppered containers. To each 100
ml of molybdate solution required for a batch of determinations add 5 ml of concentrated nitric and
filter immediately before using.
(2) Standard Alkali Solution—Dilute 324.0 ml of carbonate-free IN sodium (or potassium) hydroxide
solution to 1 liter. 50 ml of this solution should neutralize 16.20 ml of 1.000 N acid solution. Adjust the
solution if necessary, to this exact concentration. One ml of the standard alkali solution equals 1 mg of
or P205 or 1% P205 on the basis of 0.1 g. sample.
(3) Standard Acid Solution—Prepare a solution of hydrochloric or nitric acid corresponding in
concentration to the standard alkali solution. Standardize the acid solution against the standard alkali
solution using phenolphthalein as the indicator.
(4) Nitric Acid, Concentrated (67-71%).
(5) Hydrochloric Acid, Concentrated (36-38%).
(6) Perchloric Acid, (70-72%).
(7) Ammonium Hydroxide, Concentrated (28-30%).
(8) Ammonium Nitrate Solution—Dissolve 100 g. of phosphorus-free ammonium nitrate in water and dilute
to 1 liter.
(9) Nitric Acid Dilute—Add 1 volume of concentrated nitric acid to 3 volumes of water and mix well.
(10) Methyl Red Indicator Solution—Dissolve 0.1 g. of methyl red in 60 ml of alcohol 95% ethyl alcohol, or
ethyl alcohol that has been denatured with methyl alcohol.
(11) Phenolphthalein Indicator Solution—Dissolve 1 g. of phenolphthalein in 100 ml of alcohol (95% ethyl
alcohol, or ethyl alcohol that has been denatured with methyl alcohol.

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C-1.5 Preparation of Sample Solution:
equivalent purity:-
(1) Take 2ml of sample into a 250 ml beaker.
(2) Dissolve the sample in accordance with the appropriate method below, depending upon the nature of
the sample.
(a) Suitable for sample containing small quantities of organic matter—Add 30 ml of
concentrated nitric acid and 3-5 ml of concentrated hydrochloric acid to the beaker. Place a
cover glass on the beaker and boil until any organic matter present is destroyed.
(b) Suitable for fertilizer containing much iron or aluminum phosphate and for basic slag—
Add 15-30 ml of concentrated hydrochloric acid and 3-10 ml of concentrated nitric acid to
the sample beaker. Cover the beaker with a cover glass and boil until solution is complete.
(c) Suitable for all fertilizers—Before using this technique read, and become thoroughly
familiar with, the PRECAUTIONS section at the end of the method.
Transfer the weighed sample quantitatively to an Erlenmeyer flask (or kjeldahl flask preferably for
samples containing large quantities of organic matter). Add 20-30 ml of concentrated nitric acid and
boil gently for 30-45 minutes to oxidize all easily oxidizable matter. Cool the flask and add 10-20 ml
of 70-72% perchloric acid. Boil very gently until the solution is colourless, or nearly so, and dense
white fumes appear in the flask. DANGER : Do not boil to dryness at any time. With samples
containing large quantities of organic matter, the temperature should be raised to the fuming point
(about 170 ºF) over a period of at least one hour. Cool slightly, add 50 ml of water and boil for a few
minutes.
(3) Cool the sample solution and transfer it quantitatively to a 200 ml volumetric flask. Record this volume
(200 ml) as C. Dilute the solution to the mark, mix well and filter through a dry, quantitative filter
paper. Collect the filtrate in a clean flask and stopper until ready for use.
C-1.6 Procedure:
(1) Pipet into a beaker or flask an aliquot of the sample solution corresponding to 0.4 ml of sample if the
P205 content of the sample is less than 5 %, 0.2 ml of sample if the P205 content is 5-20% or 0.1 ml of
sample if the P205 or content is greater than 20%. Record the volume of the aliquot used and identify it
as E.
(2) Add 7 m, of concentrated nitric acid (or 65 ml of ammonium nitrate solution). Add concentrated
ammonium hydroxide until the precipitate that forms dissolves only slowly on vigorous stirring. If the
sample solution does not give a precipitate with the ammonium hydroxide, make the solution slightly
alkaline to limits paper with the ammonium hydroxide and then slightly acid with dilute nitric acid.
(3) Dilute the solution to 75-100 ml and adjust the temperature to 25-30 ºC.
(4) Add to the neutralized solution 20-25 ml of the molybdate solution if the P205 content of the sample is
less than 5 %, 30.35 ml If the P205 content is between 5 and 20% and enough molybdate solution to
ensure complete precipitation for P205 content greater than 20%.
(5) Place the solution in the shaking or stirring apparatus and agitate for 30 minutes at room temperature.
(6) Decent the supernatant liquid at once through a filter crucible. Wash the precipitate remaining in the
vessel twice by adding 25-30 ml portions of water, agitating thoroughly, allowing the precipitate to
settle and decanting the wash into the filter crucible. Finally, transfer the precipitate to the filter and
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wash with cold water until the filtrate from two fillings of the crucible shows no acid reaction on the
adding of two drops of methyl red solution.
(7) Transfer the crucible to a beaker and add sufficient standard alkali solution from a buret to dissolve the
precipitate, avoiding an excess of more than 3 ml Record the volume of alkali solution to the nearest
0.01 ml agaitate the beaker to dissolve all remaining particles of the precipitate.
(8) Dilute to 150 ml with water, add two drops of phenolphthalein indicator solution and titrate with the
standard acid solution to the disappearance of the pink color. Record the volume of standard acid
solution required to the nearest 0.01 ml
C-1.7 Calculation:
Calculate the phosphorus content (as P205) by the equation.
% (Vol.) P205 = A—B × C × 100

S × D × 1000
Where
A is the volume of standard alkali solution used dissolve the precipitate, in ml
B is the volume of standard acid solution required to titrate the excess alkali solution, in ml
C is the amount of sample volume taken under “preparation of sample solution”, in ml
D is the volume of the aliquot of sample solution taken in PROCEDURE, step (1) in ml
B. SPECTROPHOTOMETRIC METHOD
C-1.8 Apparatus:
(1) Spectrophotometer—with matched pair of absorption cells. The light path length of the cells should
be 1 cm. preferably, although cells up to 1.3 cm. in light path length may be used.
C-1.9 Reagents:
(1) Standard Phosphate Solution—Dry several grams of potassium hydrogen phosphate (KH2PO4),
primary standard grade, in an air oven at 105ºC for two hours. Remove from the oven and allow it to
cool in a desiccator. Accurately weigh 1.5340 g. of the dried potassium hydrogen phosphate and
dissolve in water. Transfer the solution to a 200 ml volumetric flask and dilute to the reference mark
with additional water. Stopper and mix well.
(2) Molybdovanadate Solution—Dissolve 40 g. of ammonium molybdate tetrahydrate, (NH4)6Mo7024.
4H20), in 400 ml of hot water and allow to cool. Dissolve 2 g. of ammonium vanadate, NH4VO3, in
250 ml of hot water, cool and add 450 ml of 70% perchloric acid. Gradually add the molybdate solution
to the vanadate solution with constant stirring. Dilute the final solution to 2 liters with water and mix
well.
C-1.10 Calibration:
(1) Prepare a series of calibration solution by measuring into 100-ml volumetric flasks the volumes of
standard phosphate solution, REAGENTS, (1), indicated in the table below. Measure the volumes
carefully with a burette.

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CALIBRATION
Calibration Concentration, mg. Volume of Standard

Solution P205/ml phosphate Solution,
ml
A 0.4 10.00
B 0.5 12.50
C 0.6 15.00
D 0.7 17.50
E 0.8 20.00
F 0.9 22.50
G 1.0 25.00
_______________________________________________________________
Dilute each solution to the reference mark with water and mix well.
(2) Pipet into 100-ml volumetric flasks 5-ml aliquots of the seven calibration solutions. These flasks will
contain 2, 2.5, 3.0, 3.5, 4.0, 4.5 and 5.0 mg P205. To each flask add 45 ml of water, and within five
minutes for the entire series, add 20 ml of molybdovanadate solution by pipes, dilute to the mark with
water and mix. Allow the solution to stand for 10 minutes.
(3) Fill the two absorption cells with the solution containing 2 mg P205. Set the spectrophotometer to 400
mµ and adjust to zero absorbance with one of the cells in the reference position. Move the other cell
into the light path. If a negative absorbance is obtained, reverse the position of the cells and readjust to
zero absorbance with the new cell in the light Path. Identify this cell permanently as the reference cell.
If the absorbance of the sample cell is greater than 0.001, record it as the correction factor and correct
all subsequent absorbance readings by subtracting this factor.
(4) Determine the absorbance of the other solution (2.5 through 5.0 mg. P205 retaining the 2-mg solution
in the reference cell at zero absorbance. After each determination empty and refill the reference cell
with fresh portions of the 2-mg solution to avoid any error that might arise from temperature changes.
(5) Prepare a calibration curve by plotting the observed absorbance values (corrected if necessary) against
the respective quantities of P205 in the solutions prepared in step (2) i.e. 2.0 through 5.0 mg. P205.
When the calibration work has been completed, discard the seven calibration solutions (A-G). Do not
attempt to use these solutions at a later date. The standard phosphate solutions, REAGENTS (1), may
be retained.
(1) Take 1 ml of uniform representative portion of the sample into a 250-ml beaker.
(2) Mix the sample in accordance with step (2) of PREPARATION OF SAMPLE SOLUTION section
under the VOLUMETRIC METHOD alternative.
(3) Cool the sample solution and transfer it quantitatively to a volumetric flask. If the P205 content is less
than 5% use a 250-ml volumetric flask. If the P205 content is greater than 5% dilute to such volumetric
that a 5- or 10-ml aliquot will contain 2—5 mg P205. Record the volume of the volumetric flask as V1.
Dilute the solution to the mark of the volumetric flask, mix well and filter through a dry quantitative
filter paper. Collect the filtrate in a clean flask and stopper until ready for use.

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C-1.12 Procedure
(1) Prepare fresh calibration solutions A and D by measuring accurately from a burette 10 ml and 17.50 ml
of the standard phosphate solution into 100-ml volumetric flask. Dilute each aliquot to the reference
mark with water and mix well.
(2) Pipet into 100-ml volumetric flasks 5 ml of the freshly prepared calibration solution A. Label the flask
“2 mg. P205”. Pipette into another 100-ml volumetric flask 5 ml of the freshly prepared calibration
solution D and label the flask “3.5 mg. P205”. Develop the color as under CALIBRATION step (2),
starting with the addition of 45 ml of water. Fill the reference cell with the “2 mg. P205” standard and
adjust the instrument to zero absorbance at 400 m/µ. Determine the absorbance of “3.5 mg. P205”
standard. The absorbance this standard should be practically identical with the corresponding value on
the calibration curve.
(3) Pipet a 5- or 10-ml aliquot of the sample solution from step (3) under PREPARATION OF SAMPLE
SOLUTION into a 100-ml volumetric flask. Record the volume of the aliquot used as V2. Develop the
color and determine the absorbance in the same manner as in step (2).
(4) Read and record as W, the P205 content of the sample aliquot from the calibration curve.
C-1.13 Calculation:
(1) Determine the weight of sample represented by the aliquot used for the absorbance measurement
by the equation.
SA = S ×1000 x V2
V1
Where
S is the volume of sample taken for analysis in ml
V1 is the volume, in ml to which the sample solution was diluted in step (3) of the
PREPARTION OF SAMPLE SOLTUION section.
V2 is the volume of the aliquot taken for the color development step (3) of
PROCEDURE.
SA is the volume of sample in the aliquot used for the absorbance measurement in ml.
(2) Calculate the total phosphorus content (as P205) by the equation.
% P205 = W × 100
SA
Where
W is the weight of P205 in the sample aliquot, POROCEDURE step (4) in ml.
C-1.14 Reporting:
Report the result from the volumetric or the spectrophotometric determination as:
Phosphours, Total (as P205)----------% P205 (vo1.)
Indicate in the report which alternative was used to determine the total phosphorous.

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C-1.15 Precautions:
Contact of perhloric acid solution with oxidizable combustible materials or with dehydrating or
Reducing agents may result in fire or explosion. Persons using this acid should be thoroughly familiar with its
hazards, and safety practice should include the following:
(a) Remove spilled perchloric acid by immediate and thorough washing large quantities of water.
(b) Hoods and ducts for perchloric acid vapor should be made of chemically inert materials and so design
that they can be thoroughly washed with water. The exhaust system should discharge in a safe location,
and the fan should be accessible for cleaning.
(c) Avoid use of organic chemicals in hoods employed for perchloric acid digestions.
(d) Use goggles barrier shields, and other devices as may be necessary for personnel protection.
(e) In wet combustions with perchloric acid, treat the sample first with nitric acid to destroy easily
oxidizable organic matter.
(f) Contact of perchloric acid solution with strong dehydrating agents such as phosphours pentoxide or
concentrated sulfuric acid may result in formation of explosive anhydrous perchloric acid. Exercise
special care in performing analysis requiring the use of perchloric acid with such agents.
C-2 PHOSPHORUS (WATER-SOLUBLE) CONTENT OF FERTILIZERS
C-2.1 Scope
The procedure is applicable to phosphorus—containing fertilizers such mixed fertilizers, and fertilizer raw
materials. The spectrophotometric alternative is not applicable to materials yielding colored water extracts or
water extracts containing ions other than orthophosphate which from colored complexes with molybdovanadate
and is not recommended for basic slag. The volumetric alternative may be used in all cases.
C-2.2 Summary of Method:

A water extract of the sample is analyzed for phosphate content by either a volumetric or spectrohoametric
method. The volumetric option involves precipitation of the phosphate with molydbate solution, removal of the
precipitate by filtration, dissolution of the precipitate in an excess of standard alkali solution and titration of the
excess alkali with standard acid. In the spectrophotometric alternative the sample solution is reacted with
molybdovanadate reagent and the absorbance of the resulting product measured in a spectrophotometer. The
phosphorous content is reported percent P205 to the nearest 0.01%.

equivalent purity:-
(1) Take 1ml of representative portions of the sample as S.
(2) Transfer the sample quantitatively to a folded. 9-cm, quantitative, filter paper placed in a conical
funnel. Wash the sample in the paper with small portions of room-temperature water, collecting the
filtrate in a 250-ml volumetric flask. Allow each portions to pass through the filter completely before
adding another portion. Continue the washing until the filtrate volume is approximately 240 ml Use
section if it be comes apparent that washing will not be complete within one hour. If the filtrate is
turbid, add 1-2 ml of concentrated nitric acid. Dilute the solution to the mark with water and mix
thoroughly. Record the volume of the solution as V1.

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(3) Determine the phosphate content of the water extract by one of the following procedures. If the water
extract is colored, or contains ions other than orthophosphate that will form colored complexes with
molybdovanadate, the volumetric method must be used.
C-2.4 A. VOLUMETRIC METHOD:
C-2.5 Apparatus:
(1) Agitator—A machine capable of shaking Erlenmeyer flask such as the wrist-type shaker or any device
capable of stirring the contents of a beaker, such as a magnetic stirrer, may be used.
(2) Stinered Crucible—Porcelain, 30-ml capacity, fine porosity. (Maximum pore radius, 3). Alternatively,
25-ml Gooch crucible prepared to retain fine precipitates may be used.
C-2.6 Reagents:
(1) Molybdate Solution—Dissolve 100 g of molybdic anhydride (MoO3) in a mixture of 144 ml of
concentrated ammonium hydroxide and 271 ml of water. Cool and pour the solution slowly with
constant stirring into a cool mixture of 489 ml of concentrated nitric acid and 1148 ml of water. Keep
the final mixture in a warm place for several days or until a portion heated to 40 ºC deposits no yellow
ml of molybdate solution required for a a batch of determinations add 5 ml of concentrated nitric acid
and filter immediately before using.
(2) Standard Alkali Solution—Dilute 324.0 ml of carbonate-free IN sodium (or potassium) hydroxide
solution to 1 liter. Fifty ml of this solution should neutralize 16.20 ml of IN acid solution. Adjust the
solution, if necessary to this exact concentration. One ml of the standard alkali solution equals 1 mg of
P205 or 1% P205 on the basis of 0.1 g. of sample.
(3) Standard Acid Solution—Prepare a solution of hydrochloric or nitric acid corresponding in
concentration to the standard alkali solution. Standardize the acid solution against the standard alkali
solution using phenolphthalein as the indicator. Adjust the solution, if necessary, so that 20.00 ml of the
acid is equivalent to 20.00±0.02 ml of the standard.
(4) Nitric Acid, reagent grade—69-71%.
(5) Ammonium Nitrate Solution—Dissolve 100 g. of phosphorus free ammonium nitrate in water and
dilute to 1 liter.
(6) Ammonium Hydroxide, reagent grade—28-30%.
(7) Methyl Red Indicator Solution—Dissolve 0.1g. methyl red in 50 ml of alcohol (95% methyl alcohol,
or ethyl alcohol that has been denatured with methyl alcohol). Dilute to 100 ml with water and mix
well.
(8) Phenolphthalein Indicator Solution—Dissolve 1 g. or phenolphthalein in 100 ml of alcohol (95%
ethyl alcohol, or ethyl alcohol that has been denatured with methyl alcohol).
C-2.7 Procedure:
(1) From the sample solution obtained in PREPARATION OF SAMPLE SOLUTION step, (2) pipet an
aliquot that will contain 20-40 mg. of P205 into a beaker or flask, record the volume of the aliquot as
V2.
(2) Add 10 ml of concentrated nitric acid (or 65 ml of ammonium nitrate solution to the sample aliquot.
Carefully add concentrated ammonium hydroxide until the precipitate that forms dissolves only slowly
on vigorous stirring.

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(3) Dilute the solution to 75-100 ml and adjust the temperature to 25-30 C. If the sample solution does not
give precipitate with the ammonium hydroxide in step (2) make the solution slightly alkaline to litmus
paper with the ammonium hydroxide and then slightly acid with dilute nitric acid.
(4) Add the neutralized solution 20-30ml of the molybdate solution. Allow the precipitate to settle
momentarily and test for completeness of precipitation by adding 1 ml of molybdate solution to the
clear, supernatant liquid. If a precipitate forms, continue to add molybdate solution until precipitation is
complete. Place the solution in the shaking or stirring apparatus agitate for 30 minutes at room
temperature.
(5) Decant the supernatant liquid at once through a filter crucible. Wash the precipitate remaining in the
vessel twice by adding 25 to 30 ml portions of water, agitating thoroughly, allowing the precipitate to
settle, and decanting the wash water into filter crucible. Finally, transfer the precipitate to the filter and
wash with boiled water, until the filtrate from two fillings of the crucible shows no acid reaction on the
addition of two drops of methyl red indicator.
(6) Transfer the crucible to a beaker and add sufficient standard alkali solution form a buret to dissolve the
precipitate, avoiding an excess of more than 3 ml Record the volume of alkali solution to the nearest
0.01 ml Agitate the beaker to dissolve all remaining particles of the precipitate.
(7) Dilute to 150 ml with water, add two drops of phenolphthalein solution and titrate with the standard
acid solution to the disappearance of the pink color. Record the volume of standard acid solution
required to the nearest 0.01 ml
C-2.8 Calculation:
Calculate the concentration of water-soluble phosphorus in the sample as:
% P205 = (A-B) × V1 × 100

S × V2 × 1000
A is the volume of standard alkali solution used to dissolve the precipitate, in ml

B is the volume of standard acid solution required to titrate the excess alkali solution in ml
V1 is the volume of the sample solution from PREPARATION OF SAMPLE SOLUTION, step (2) in ml
S is the volume of sample, PREPARATION OF SAMPLE SOLTUION, step (1) in ml
V2 is the volume of the aliquot of sample solution taken in PROCEDURE, step (1) in ml
B. SPECTROPHOTOMETRIC METHOD
C-2.9 Apparatus:
(1) Spectrophotometer—with matched pair of absorption cells. The light path of the cells should be 1 cm.
preferably, although cells up to 1.3 cm. in light path length may be used.
C-2.10 Reagents:
(1) Standard Phosphate Solution—Dry several grams of potassium hydrogen phosphate, KH2PO4),
primary standard grade, in an air oven at 105ºC. for two hours. Remove from the oven and allow to
cool in a desiccators. Accurately weigh 1.5340 g. of the dried potassium hydrogen phosphate and
dissolve in water. Transfer the solution to a 200-ml volumetric flask and dilute to the reference mark
with addition water Stopper and mix well.
SDC/ PSQCA
PS: 5469-2020
(2) Molybdovanadate Solution—Dissolve 40 g. of ammonium molybdate tetrahydrate, (NH4)6 MO7O24

4H2O, in 400 ml of hot water and allow to cool. Dissolve 2 g of ammonium vanadate NH4 VO3 in 250
ml of hot water, cool and add 250 ml of 70% perchloric acid. Gradually add the molybdate solution to
the vanadate solution with constant stirring dilute the final silution to 2 liters with water and mix well.
C-2.1 Calibration
(1) Prepare a series of calibration solutions by measuring into 100 ml volumetric flasks the volumes of
standard phosphate solution REAGENTS, (1) indicated in the table below: Measure the volumes
Calibration Solution Concentration Volumes of Standard

mg. P205 /ml Phosphate Solution ml
A 0.4 10.00
B 0.5 12.50
C 0.6 15.00
D 0.7 17.50
E 0.8 20.00
F 0.9 22.50
G 1.0 25.00
(2) Pipet into 100 ml volumetric flaks 5 ml aliquots of the seven calibration solutions. These flasks will
contain 2, 2.5, 3.0, 3.5, 4.0, 4.5 and 5.0 mg. P205. To each flask add 45 ml of water and within five
minutes for the entire series, add 20ml of molybdovanadate solution by pipette, dilute the marks with
water and mix. Allow the solution to stand for ten minute.
(3) Fill the two absorption cells with the solution containing 2 mg P205. Set the spectrophotometer to 400
mµ and adjust to zero absorbance with one of the cells in the reference position. Move the other cell
into the light path. If a negative absorbance is obtained, reverse the position of the cells and readjust to
zero absorbance with the new cell in the light Path. Identify this cell permanently as the reference cell.
If the absorbance of the sample cell is greater than 0.001, record it as the correction factor and correct
all subsequent absorbance readings by subtracting this factor.
(4) Determine the absorbance of the other solution (2.5 through 5.0 mg. P205 retaining the 2-mg solution
in the reference cell at zero absorbance. After each determination empty and refill the reference cell
with fresh portions of the 2-mg solution to avoid any error that might arise from temperature changes.
the respective quantities of P205 in the solutions prepared in step (2) i.e. 2.0 through 5.0 mg. P205.
When the calibration work has been completed, discard the seven calibration solutions (A-G). Do not
attempt to use these solutions at a later date. The standard phosphate solutions, REAGENTS (1), may
be retained.

SDC/ PSQCA
PS: 5469-2020
C-1.12 Procedure
(1) Prepare fresh calibration solutions A and D by measuring accurately from a burette 10 ml and 17.50 ml
of the standard phosphate solution into 100-ml volumetric flask. Dilute each aliquot to the reference
mark with water and mix well.
(2) Pipet into 100-ml volumetric flasks 5 ml of the freshly prepared calibration solution A. Label the flask
“2 mg. P205”. Pipette into another 100-ml volumetric flask 5 ml of the freshly prepared calibration
solution D and label the flask “3.5 mg. P205”. Develop the color as under CALIBRATION step (2),
starting with the addition of 45 ml of water. Fill the reference cell with the “2 mg. P205” standard and
adjust the instrument to zero absorbance at 400 m/µ. Determine the absorbance of “3.5 mg. P205”
standard. The absorbance this standard should be practically identical with the corresponding value on
the calibration curve.
(3) Pipet a 5- or 10-ml aliquot of the sample solution from step (3) under PREPARATION OF SAMPLE
SOLUTION into a 100-ml volumetric flask.
(4) Record the volume of the aliquot used as V2.
(5) Develop the color
(6) Determine the absorbance in the same manner as in step (2).
(7) Read and record as W, the P205 content of the sample aliquot from the calibration curve.
C-2.13 Calculation:
(1) Determine the weight of sample represented by the aliquot used for the absorbance measurement by the
equation
SA=S X 1000 X V2 x V3
V1 x V4
Where
S is the weight of sample taken for analysis, in g.

V1 is the volume of the sample solution from PREPARAT1ON OF SAMPLE SOLUTION, step
(2) in ml .
V2 is the volume of the aliquot from PROCEDURE, step (5) in ml. *
V3 is the volume of the aliquot from PROCEDURE, step (3) in ml.
V4 is the volume of the diluted solution in CEDURE, stop (3) in ml.
SA is the weight of sample in the aliquot used for the absorbance measurements, in mg. Omit terms
V3 and V4 from the calculation if no dilution o the sample solution was required.
(2) Calculate the concentration of water—soluble P2O5 in the sample as :
% Water—Soluble Phosphorus (as P205) = W X 100

SA
Where W is the weight of P205 in the aliquot taken for the absorbance measurement in PROCEDURE, step (7)
in mg.
C-2.14 Reporting:
Report the concentration of water-soluble phosphorus (as P205) as :

SDC/ PSQCA
PS: 5469-2020
Water-Soluble Phosphorus (AM—S 600.46) (%P205)
Indicate in the report which alternative procedure was used to obtain the result.
C-3 CITRATE—INSOLUBLE P205 AND AVAILABLE P205 IN FERTILIZER
C-3.1 Scope :
The procedure is applicable to phosphorus-containing liquid fertilizers and fertilizer raw materials. The
spectrophotometric alternative is not applicable to materials yielding colored solutions or solutions
containing ions other than orthophosphate which form colored complexes with molybdovanadate, nor is it
recommended for basic slag. The volumetric method may be used in all cases.
C-3.2 Summary of Method:
A sample of the fertilizer is successively extracted with water and ammonium citrate solution. The latter
extraction is carried out under prolonged agitation at an elevated temperature. After filtration and ignition, the
residue is dissolved and the solution is analyzed for P205 content by either a spectrophotometric or
volumetric method. In the spectrophotometric alternative the sample solution is reacted with molybdovanadate
reagent and the absorbance of the resulting product measured in a spectrophotometer. The volumetric option
involves precipitation of the phosphate with molybdate solution, removal of the precipitate by filtration,
dissolution of the precipitate in an excess of standard alkali and titration of. the excess alkali with standard acid.
The per cent citrate-insoluble P2O5 is calculated and reported as per cent of the original sample. Available
P2O5 is calculated as the difference between the % citrate-insoluble P2O5 and the % total P2O5 (C-1) and
reported as per cent of the original sample.
C-3.3 Apparatus:
Shaking Machine—capable of shaking 250-m1. Volumetric flasks while maintaining them at a temperature of
65+ 2°C. for two hours. A wrist-type shaker positioned so that one arm enters an opening in the side of an air
oven that is held at 35°C. is a suggested arrangement.
C-3.4 Reagents:
References to water in this and the following sections shall be understood to mean distilled water, or water of
equivalent purity:—
Ammonium Citrate Solution.—Dissolve 37 g. of crystallized citric acid in 14- liters of water and nearly
neutralize by adding 345 ml. of concentrated ammonium hydroxide (28-29 % NH3). If the concentration of
ammonia is less than 28 %, add a correspondingly larger volume and dissolve the citric acid in a
correspondingly smaller) volume of water. Cool and adjust the pH of the solution to 7.0 by adding, carefully.
small portions of ammonium hydroxide. Mix thoroughly and measure the neutrality of the solution after each
addition with a pH meter. Dilute solution if necessary to specific gravity 1.09 at 20°C. The volume should be
about 2 liters. Store the solution in tightly stoppered bottles and check pH from time to time.

(1) Take 1ml of representative portion of the sample.

SDC/ PSQCA
PS: 5469-2020
(2) Transfer the sample quantitatively to a 9-cm, folded filter paper in a funnel and wash with successive
small portions of water until the volume of filtrate is about 225 ml. Allow each portion of wash water to
pass through the filter before adding more water. Use suction if after 30 minutes, it is obvious that the
filtration cannot be completed in one hour.
(3) Within one hour transfer the filter paper containing the water-insoluble residue to a 250-m1.
Volumetric flask and add 100-m1. of the ammonium citrate solution previously heated to 65°C. Close
the flask with a smooth rubber stopper, shake vigorously to disintegrate the paper. Relieve the pressure
by re-moving the stopper momentarily. Replace the stopper tightly and clamp the flask in the shaking
machine. Shake the flask for one hour while maintaining its temperature at 65°C. in the oven. Shaking
should be vigorous enough so that the sample is dispersed throughout the solution and so that the entire
interior of • the flask and the underside of the stopper are continually in con-tact with the solution.
(4) At the end of the 1 hour agitation, remove the flasks from the shaker and filter the contents immediately
by suction as rapidly as possible on a dry, quantitative filter paper (Whatman —5 or equivalent).. The
paper may be placed in a Buchner funnel or in a conventional funnel using a platinum of other cone to
support the paper. Wash the residue with water at 65°C. until the volume of the filtrate is about 350 ml.
Allow time for thorough draining before adding more water. If the material is of the type that will yield
a cloudy filtrate, wash the residue with 5 % -ammonium nitrate solution in place of the hot water.
(5) Dry the filter paper and contents carefully, being …
A. SPECTROPHOTOMETRIC METHOD
C-2.9 Apparatus:
(1) Spectrophotometer—with matched pair of absorption cells. The light path of the cells should be 1 cm.
preferably, although cells up to 1.3 cm. in light path length may be used.
C-2.10 Reagents:
(1) Standard Phosphate Solution—Dry several grams of potassium hydrogen phosphate, KH2PO4),
primary standard grade, in an air oven at 105ºC. for two hours. Remove from the oven and allow to
cool in a desiccators. Accurately weigh 1.5340 g. of the dried potassium hydrogen phosphate and
dissolve in water. Transfer the solution to a 200-ml volumetric flask and dilute to the reference mark
with addition water Stopper and mix well.
(2) Molybdovanadate Solution—Dissolve 40 g. of ammonium molybdate tetrahydrate, (NH4)6 MO7O24
4H2O, in 400 ml of hot water and allow to cool. Dissolve 2 g of ammonium vanadate NH4 VO3 in 250
ml of hot water, cool and add 250 ml of 70% perchloric acid. Gradually add the molybdate solution to
the vanadate solution with constant stirring dilute the final silution to 2 liters with water and mix well.
C-2.1 Calibration
(1) Prepare a series of calibration solutions by measuring into 100 ml volumetric flasks the volumes of
standard phosphate solution REAGENTS, (1) indicated in the table below: Measure the volumes

SDC/ PSQCA
PS: 5469-2020
Calibration Solution Concentration Volumes of Standard

mg. P205 /ml Phosphate Solution ml
A 0.4 10.00
B 0.5 12.50
C 0.6 15.00
D 0.7 17.50
E 0.8 20.00
F 0.9 22.50
G 1.0 25.00
(2) Pipet into 100 ml volumetric flaks 5 ml aliquots of the seven calibration solutions. These flasks will
contain 2, 2.5, 3.0, 3.5, 4.0, 4.5 and 5.0 mg. P205. To each flask add 45 ml of water and within five
minutes for the entire series, add 20ml of molybdovanadate solution by pipette, dilute the marks with
water and mix. Allow the solution to stand for ten minute.
(3) Fill the two absorption cells with the solution containing 2 mg. P2O5. Set the spectrophotometer to 400
m/micron and adjust to zero absorbance with one of the cells in the reference position. Mae the other
cells into the light path. If a negative absorbance is obtained, reverse the position of the cells and
readjust to zero absorbance with the new cell in the reference position. Identify this cell permanently as
the reference cell. If the absorbance of the sample cell is greater than 0.001, record it as the correction
factor and correct all subsequent absorbance readings by subtracting this factor.
(4) Determine the absorbance of the other solution (2.5 through 5.0 mg.) (P2O5), retaining the 2-mg.
solution in the reference cell at zero absorbance. After each determination empty and refill the
reference cell with fresh portions of the 2-mg. solution to avoid any error that might arise from
temperature changes.
the respective quantities of P2O5 in the solutions prepared in step (2), i.e. 2.0 through 5.0 mg. P2O5.
When the calibration work has been completed, discard the 7 calibration solutions (A to G). Do not
attempt to use these solutions at a later date. The standard phosphate solution [REAGENTS (1)] may be
retained.
C-3.10 Procedure:
(1) Prepare fresh calibration solutions A and D by mea-suring accurately from a buret 10.00 ml. and 17.50
ml. of the standard phosphate solution into 100 ml. volumetric flasks. Dilute each aliquot to be
reference mark with water and mix well.
(2) Pipet into a 100-m1. volumetric flask, 5 ml. of the freshly, prepared calibration solution A. Label the
flask "2 mg. P2 05" Pipet into another 100 ml. volumetric flask 5 ml. of the freshly prepared calibration
solution D and label the flask "3.5 mg. P2 05. Develop the color as under CALIBRATION., step (2),
starting with the addition of 45 ml. of water. Fill the reference cell with the " 2 mg. P2 05 " standard
and adjust the instrument to zero absorbance at 400 m/micron Determine the absorbance of the "3.5 mg.
P2 05 " standard. The absorbance of this standard should be practically identical with the corresponding
value on the calibration curve.
(3) Pipet a 5- or 10-m1. aliquot of the sample solution from step (6) PREPARATION OF SAMPLE
SOLUTION, into a 100 ml. volumetric flask. Record the volume of the aliquot as IT2, add 45 ml. of
water to the flask and, within 5 minutes add 20 ml. of molybdovanadate solution from a pipet. Dilute to
the mark with water and mix. Allow the solution to stand 10 minutes.
SDC/ PSQCA
PS: 5469-2020
(4) Fill the reference cell with a fresh portion of the "2 mg. P2O5" solution and adjust the
spectrophotometer, if necessary, to zero absorbance. Fill the sample cell with the reacted sample
solution from step (3) and determine its absorbance at 400 m/micron
(5) Read, and record as W, the P2 05 content of the sample aliquot from the calibration curve.
C-3.11 Calculation:
(1) Determine the weight of sample represented by the aliquot used for the absorbance
measurement by the equation.
SA= S X 1000 X V2
V1
Where
S is the weight of sample taken for analysis, in g.
VI is the volume of the solution of citrate-insoluble material, PREPARATION OF SAMPLE SOLUTION,
Step (6) in ml.
V2 is the volume of the aliquot taken for the color development PROCEDURE, step (3) in ml.
SA is the weight of sample in the aliquot used for the color development, in mg.
(2) Calculate the concentration of citrate-insoluble phosphorus in the sample as:
% P2O5 = W X 100
SA
Where
W is the weight of P205 in the sample aliquot, PRO-CEDURE, step (5), in mg.
C-3.12 B. VOLUMETRIC METHOD
C-3.13 Apparatus :
(1) Agitator.—A machine capable of shaking Erlenmeyer flasks such as the wrist-type shaker or any device
capable of stirring the contents of a beaker, such as a magnetic stirrer, may be used.
(2) Filter Crucible.—Porcelain, 30 mt. capacity, fine porosity. A suitable item is Selas crucible No. 3001.
Alternatively, 25-m1. Gooch crucibles prepared to retain fine precipitates may be used.
C-3.14 Reagents:
(1) Molybdate Solution.—Dissolve 100g. of molybdic anhydride (Mo03) in a mixture of 144 ml. of
concentrated ammonium hydroxide and 271 ml. of water. Cool and pour the solution slowly, with
constant stirring into a cool mixture of 489 ml. of concentrated nitric acid and 1148 ml. of water. Keep
the final mixture in a warm place for several days or until a portion heated to 40'C. deposits no yellow
ml. of molybdate solution required for a batch of determinations add 5 ml. of concentrated nitric acid
and filter immediately before using.
(2) Standard Alkali Solution.—Dilute 324.0 ml. of carbonate-free, IN sodium (or potassium) hydroxide
solution to 1 liter. 50 ml. of this solution should neutralize 16.20 ml. of IN acid solution. Adjust the
solution, if necessary, to this exact concentration. 1 ml. of the standard alkali solution equals 1 mg. of
P2 05, or 1% P2 05 on the basis of a 0.1 g. sample.
SDC/ PSQCA
PS: 5469-2020
(3) Standard Acid Solution.—Prepare a solution of hydrochloric or nitric acid corresponding in

concentration to the stand-ard alkali solution. Standardize the acid solution against the standard
alkali solution using phenolpthalein as the indicator. Adjust the solution, if necessary, so that 20.00
ml. of the acid is equivalent to 20.00 +0.02 ml. of the standard alkali.
(4) Nitric Acid, Concentrated (69-71%3):
(5) Ammonium Nitrate Solution.—Dissolve 100 g. of phosphorus-free ammonium nitrate in water and
dilute to 1 liter.
(6) Ammonium- Hydroxide,
(7) Methyl Red Indicator methyl red in 60 ml. of alcohol that has been denatured Concentrated (28—.30 :
Solution.—Dissolve 0.1 g. of (95% ethyl alcohol, or ethyl with methyl alcohol).
(8) Phenolphthhalein Indicator Solution.—Dissolve 1 g. of phenolphthalein in 100 ml. of alcohol (95%
ethyl alcohol, or ethyl alcohol that has been denatured with methyl alcohol). "
C-3.15 Procedure:
(1) To the sample solution from PREPARATION OF SAMPLE SOLUTION, step (7) add 5 ml. of
concentrated nitric acid (or 65 ml. of ammonium nitrate solution). Carefully add concentrated
ammonium hydroxide until the precipitate that forms dissolves only slowly on vigorous stirring.
(2) Dilute the solution to 75-100 ml. and adjust the temperature to 25-30°C. If the sample solution does not
give a precipitate with the ammonium hydroxide in .step (1) make the solution slightly alkaline to
litmus paper with the ammonium hydroxide and then slightly acid with dilute nitric acid:
(3) Add to the neutralized solution 20-25 ml. of the molybdate solution. Place the solution in the shaking or
stirring apparatus and agitate for 30 minutes at room temperature.
(4) Decant the supernatant liquid at once through a filter crucible. Wash the precipitate remaining in the
vessel twice by adding 25 to 30 ml. portions of Water, agitating thoroughly, allowing the precipitate to
settle and decanting the wash water into the filter crucible. Finally transfer the precipitate to the alter
and wash with cold water until the filtrate from two fillings. of the crucible shows no acid reaction on
the addition of two drops of methyl red indicator.
(5) Transfer the crucible to a beaker and add sufficient standard alkali solution from a buret .to dissolve the
precipitate avoiding an excess of more than 3 ml. Record the volume of alkali solution to the nearest
0.01 ml . Agitate the beaker to dissolve all remaining particles of the precipitate.
(6) Dilute to 150 ml with water, add two drops of phenolphthalein indicator solution and titrate with the
standard acid solution to the disappearance of the pink color. Record the volume of standard acid
solution to the nearest 0.01 ml.
C-3.16 Calculation:
Calculate the concentration of citrate-insoluble phosphorus in the sample as under:
% P205 = (A-B) X 100

S X 1000
Where
A is the volume of standard alkali solution used to dis-solve the precipitate, in ml.
B is the volume of standard acid solution required to titrate the excess alkali solution in ml.
S is the weight of sample used (PREPARATION OF SAMPLE SOLUTION) step (1), in g.

SDC/ PSQCA
PS: 5469-2020
C-3.17 Reporting:
Report the concentration of citrate-insoluble phosphorus (as P205) as :
Citrate-Insoluble Phosphorus -------------------------% P205 (Vol.)
indicate in the report which alternative was used to determine the citrate-insoluble phosphorus by inserting an A
in the parentheses after % P 05 for the spectrophotometric method or a B for the volumetric procedure. If " per
cent available phosphorus " is required by the specifications or the sample submitter, subtract the % citrate-
insoluble P205 from the % total P205 ( as determined by C— 1) and report the difference as
Available Phosphorus -----------------------% P205 (Vol.)
APPENDIX 'D'
D-1 POTASSIUM CONTENT OF FERTILIZERS
D-1.1 Scope:
The procedure is intended for the determination of soluble potassium in liquid fertilizers.
D-1.2 Summary of Method :

In the volumetric procedure the potassium salts are extracted from a portion of the sample and the
potassium precipitated with a measured volume of sodium tetraphenylhoron. The excess reagent is titrated
with a standard quaternary ammonium chloride solution. The flame photometric method involves a similar
extraction of the sample which is followed by passing the extract through an ion exchange column to re-move
interfering anions. The treated solution is aspirated into a flame photometer and the emission intensity at 767
m/micron is measured. Results are calculated as per cent K2O and re-ported to the, nearest 0.1 %.
D-1.3 Precision :
Duplicate results obtained by th same operator should not be considered suspect unless they differ by more than
the following amounts at the indicated concentration level :
% K2O Level Sodium tetraphenylboron Method Fine Photometric Method

8 -12 % 0.48 0.79
30% 0.26 1.6
60% 1.3 2.2
A. SODIUM TETRAPHENYLBORON MFTHOD
D-1.4 Reagents :
References to water in this and the following sections shall be understood to mean distilled water, or water of
equivalent purity :—

SDC/ PSQCA
PS: 5469-2020
(1) Ammonium Oxalate Solution. 4 %. — Dissolve 4+0.1 g. of ammonium oxalate, ( NH4)2 C2 04. H2O,
in 100 ml. of water.
(2) Sodium Hydonoxide Solution.. 20%. — Dissolve 20± 0.1 g. of sodium hydroxide in 100 ml. of water,
(3) Formaldehyde Solution, 37 % (Wt.).—Available in this concentration from most chemical supply
companies.
(4) Standard Quaternary Ammonium Chloride Solution.—Dilute 50 ml. of 12.8 % Zephiran chloride
(Alkyl-dimethyl Benzyl Ammonium Chloride) to 1 liter with water and mix. The concentration of the
resulting solution will be approximately 0.625 %. Cetyltrimethyl ammonium bromide
(hexadecyltrimethylammonium bromide) available from most chemical supply companies may be
substituted for the Zephiran chloride. If the bromide compound is used, dissolve 6.2±0.1 g. in water and
dilute to 1 liter with additional water.
Standardize the solution as follows.
Pipet 2.00 nil. of the unstandardised sodivut tetraphenylboron solution (STPB), REAGENTS (5) into a
125 ml. Erlenmeyer flask and add 20-25 ml. of water. 'Pipet 1 ml. of 20 % sodium hydroxide, 2.5 ml. of
37 % formaldehyde solution and 1.5 ml. of 4 % ammonium oxalate into the flask and add 6-8 drops of
Clayton yellow indicator solution. Titrate the solution with the quaternary ammonium chloride reagent
to the pink end point, using a 10 ml. buret graduated in 0.05 ml. subdivisions. Adjust the concentration
of the quaternary ammonium chloride, solution so that 2.00±0.02 ml. of the STPB solution. The
solution is relatively stable. Normally this ratio should be checked every two weeks and adjustments
made as required.
(5) Standard Sodium Tetraphenylboron Solution.—Dissolve 12 g. of sodium tetraphenylboron, NaB (C6 Hs)4,
in approximately 800 ml. of water. . Add 20-25 g. of aluminum hydroxide, Al (OH)3, stir for 5 minutes
and filter through filter paper (Whatman # 42, or equivalent) into a 1 liter volumetric flask. Rinse the
beaker spar-ingly with water and add the washings to the filter, collecting the filtrate in the volumetric
flask. Add 2 ml. of 20% sodium hydroxide solution to the filtrate, dilute to the mark with water and mix
well. Allow the solution to stand for 48 hours and standardize in the following manner.
Dissolve 2.500 g. of primary-standard grade potassium 13.3droge phosphate, KH2PO4, in water and transfer to
a 250-ml. volumetric flask. Add 50 ml. of 4 % ammonium oxalate solution, dilute to the mark with water and
mix. Transfer a 15 ml. aliquot (equivalent to 52.87 mg. K2O, or 43.88 mg. K) to' a• 100 ml. volumetric flask.
Pipet 2 ml. of 20 % sodium hydroxide solution and 5 ml. of 37 % formaldehyde solution into the flask.
Carefully transfer 43.00 ml. of the sodium tetraphenylboron (STPB) solution from a buret into the flask. Dilute
the solution to the reference mark with water and mix thoroughly. Allow the solution to stand for 5-10 minutes
and filter through a dry filter paper. Pipet a 50-m1. aliquot of the filtrate into a 125-m1. Erlenmeyer flask, add
6-8 drops of Clayton yellow indicator solution and titrate the excess STPB with the standardized quaternary
ammonium chloride solution to the pink end point:
Calculate the titer of the solution by the equation.
F = 34.58
A—B
where
A is the volume of STPB solution added (= 43.00 ml.)
B is the volume of quaternary ammonium chloride solution required to titrate the excess STPB, in
ml. F is the titer, expressed as % K20/ml. of STPB. The factor F applies only when 2.5 g. of
sample has been diluted to 250 ml. and a 15-m1. aliquot taken for the titration.
(6) Clayton Yellow Indicator Solution, 0.04 %.--Dissolve 40 mg. of Clayton yellow in 100 ml. of water. This
compound is listed as Titan Yellow in some chemical catalogs.
SDC/ PSQCA
PS: 5469-2020
D-I.5 Procedure:
(1) Take 2.5ml of representative portion of the sample. Transfer the sample quantitatively to a 250-ml.
volumetric flask. If the K2O content of the sample is known.to be greater than 50%, weigh out
1.250±0.001 g. of sample instead o f the 2.500 g.
(2) Add 50 ml. of 4 % ammonium oxalate and 125 ml. of water to the flask and boil the contents for 30
minutes. Agitate the flask occasionally during the early stage of the heating to make sure that the
sample has not caked on to the bottom .of the flask.
(3) Allow the solution to cool, dilute to the mark on the flask with water and mix thoroughly. Filter the
solution through dry filter paper (Whatman # 5, or equivalent) or allow the solution to stand until clear.
(4) Pipet a 15 ml aliquot of the clear solution into a 100 ml. volumetric flask. Pipet 2 ml. of 20 % sodium
hydroxide and 5 ml. of 37.% formaldehyde solution into the flask. Using a buret, carefully measure into
the solution 1 ml. of the STPB solution for each 1 % 1K20 expected in the sample. Mea-sure an
additional 8 mi. of the STPB solution into the flask and record to the nearest 0.01 ml. the total volume
of STPB used. Do not swirl or attempt to mix the solution in the volumetric flask while the STPB is.
being used. Intense foaming may occur making it virtually impossible to bring the volume accurately to
the reference mark. After the addition of the STPB, dilute to the mark with water and then mix
thoroughly. .
(5) Allow the solution to stand for 5-10 minutes and filter through a dry filter paper (Whatman 2.4 $, or
equivalent). (6) Pipet 50 ml. of the filterate into a 125 ml. Erlenmeyer flask, add 6-8 drops of the
Clayton yellow indicator solution and titrate with the quaternary ammonium chloride solution to the
pink end point. Record the volume of titrant required to the nearest 0.01 ml.
D-1.6 Calculation:
(1) Calculate the concentration of potassium (as 1(20) in the samples as follows :
"Potassium ( % K20) 7(9-D) F"
where
C is the volume of STPB added in step (4), in ml.
D is the volume of quaternary ammonium chloride required to titrate the excess STPB in step (6) in ml. F is the
titer of the STPB solution, in % 1(2Oiml, 4ultiply the result by .2 if a 1.25 g. sample was used.
D-1.7 B. FLAME PHOTOMETRIC METHOD
D-1.8 Apparatus:
References to water in this, and the following, sections shall be understood to mean distilled water, or water of
equivalent purity :—
(1) Flame Photometer
(2) Ion Exchange Column.—made from a' 12 inch length of 2.5 cm O.D., No. 4 rubber stoper through
which is inserted a 2-way stopcock or glass tubing connected to rubber tubing over which is placed a
compressor clamp. See Fig..1 for details of construction. Do not allow the stopcock tubing to protrude
above the stop-per. The stopper should be large enough so that there is no space between the stopper
vertex and the column wall. insert a glass wool plug in the bottom of the column. Prepare the resin
according to the following instructions. Place about 1.5 lb. of anion exchange resin in a 4-liter beaker
and add enough 5 % sodium hydroxide solution (2-3 liters) to completely float the resin when it is
being stirred. Stir the mixture With an electric stirrer for 30 minutes. Let the resin settle and decant the
sodium hydroxide solution from the beaker. Repeat the treatment with 5 % sodium hydroxide solution
SDC/ PSQCA
PS: 5469-2020
two more times, decanting the solution from the resin after each treatment. Add 3 liters of water to the
resin, stir for a few minutes, allow the resin to settle and decant the wash water. Repeat the water
washing three or four times. The resin is now in the free base form. Regenerate the resin to the nitrate
form by treating it three times with 5 % nitric acid, using the same technique as with the sodium
hydroxide solution. Wash the resin with water until the washings reach a pH of 2 or higher by stir-ring
and decanting in a large beaker. Keep the resin damp during storage. To fill the column, transfer a
suitable quantity of the prepared resin to a beaker and add enough water to suspend the solid while the
mixture is being swirled. Transfer small portion of the agitated mixture to the column, allowing the
water. to drain through the open stopcock before adding the following portion. Continue the additions,
slowly and carefully so as to avoid any pockets, until the resin bed has reached a height of' 8 inches
when the water has drained off. Wash down any resin particles clinging to the walls above the resin
bed. Fill the column with water and close the stopcock so that the water level remains above the top of
the resin bed.
D-1.9 Reagents :
(1) Ammonium Carbonate Solution.—Dissolve 50 g. or ammonium carbonate in 1 liter of water.

(2) Methyl Red Indicator Solution.—Dissolve 0.2 g. of methyl red in 100 ml. of 95 % ethyl alcohol or
ethyl alcohol that has been denatured with methyl alcohol.
(3) Dilute Nitric Acid.—Mix 1 volume of reagent grad; nitric acid (69-71 %) with 10 volumes of water.
(4) Anion. Exchange Resin.—Any one of the following • resins, or their equivalent may be used ;
Aniberlite IR-4B (Fischer Scientific Co,, Pittsburg, Pa) Doulite A-7 or Dwolite A-41. (Resinoms
Products Co.) Redwood City, California, De. Acidite _ or .Permutit-S (Permutit Inc.., 50 W 44th St.
New York 36 N. Y.),
(5) Potassium Nitrate (or Potassium Chloride).--Recrystallize the reagent grade salt twice from water and
dry for 5- hours at 105C.
(6) Sodium Hydroxide, 5 Dissolve 50 g. of reagent grade sodium hydroxide in 1 liter of water.
(7) Nitric Acid, 5 %.--Add 50 ml. of reagent grade nitric acid (69-71 %) to 1 liter of water and mix well.
D-1.10 Calibration :
(1) Dissolve 1.2931 g. of potassium nitrate (or 0.9535 g. of potassium chloride in water and dilute to 500
ml. in a volumetric flask. Mix well. This stock solution contains 1000 ppm of potassium.
(2) Prepare calibration solutions by accurately pipeting 0, 1, 2, 3, 4, 5, 6, 7 and 8 ml. of the 1000-ppm stock
solution into 100 ml. volumetric flasks. If an internal standard type of flame photometer is to be used
add the appropriate amount of lithium nitrate to each of the 9 flasks, Dilute the contents. of each flask
to the reference mark with water and .mix thoroughly. The flasks will contain 0, 10, 20, 30, 40, 50, 60,
70 and 80 ppm of potassium, respectively.
(3) Following the instructions of the manufacturer allow • the photometer to warm up, light the burner and
make the necessary adjustments, the wavelength dial (element selector on certain instruments) for
potassium (767 in/micron). Aspirate. the .50 ppm calibration solution into the flame and adjust the
wavelength dial until the maximum response is achieved.
(4) Continue to aspirate the 50 ppm calibration solution' into the name and adjust the instrument so that the
per cent transmission is 50 % (or the met' reading is at ,mid-scale). Note the temperature of the
calibration solution in the volumetric flask. The temperature of the remaining calibration solutions and
all subsequent sample solutions just prior to aspiration should be the same (+_ 2°C). (5) Determine the
per coat transmission (or meter reading) for the remaining calibration solutions. Plot the observe values
SDC/ PSQCA
PS: 5469-2020
against the corresponding concentrations, in ppm. Prepare a standard curve of emission by plotting the
observed values against the corresponding concentrations, as ppm on linear paper,
D-1.11 Procedure
(1) Weigh 1.50 ml of a uniform representative portion of the sample.

(2) Transfer the sample quantitatively to a 250-ml. volumetric flask (500 ml.) flask if the sample contains
more than 30 % K20), and add 100 ml. of water followed by 20 ml. of ammonium carbonate solution.
Boil the solution for five minutes and cool to room temperature. Dilute the solution to the reference
mark with water, mix well and filter thorough a dry filter paper (Watman #/l, or equivalent). Collect the
filtrate in a clean, dry container. Stopper the container until ready for use.
(3) Pipet 10 ml. of the filtered sample solution into a 250 ml. beaker. Add 1 drop of methyl red indicator
and neutralize the solution to the pink end point with dilute nitric acid.
(4) Adjust the water level in the ion exchange column so that it is level with the top of the resin. Transfer
the neutralized sample aliquot quantitatively to the column. Open the stop-cock carefully to give a flow
rate of 2 drops/second, collecting the 'effluent in a 250 ml. volumetric flask. Wash the sample solution
into the column with 2-3 small portions of water.
(5) Collect 50-75 ml. of effluent in the flask. Open the stopcock and collect an additional 100 ml, of
effluent while pouring water into the top of the column making certain that the water level does not fall
below the top of the resin bed. Close the stopcock and dilute the effluent in the volumetric flask to the
reference mark with water. If an internal standard instrument is being used, add an amount of lithium
nitrate equal to that used in the calibration :before diluting the effluent to volume.
(6) Check the instrument conditions and adjustments by aspirating several of the calibration solutions into
the burner and comparing the emission readings with those of the calibration curve. Make any
necessary adjustments so that the observed values agree with those on the calibration curve. This step
should be performed each day that the instrument is used.
(7) Aspirate the treated sample solution into the flame and measure the emission in the same manner as
under CALIBRA-TION. Record the per cent transmission (or dial reading).
(8) Obtain the corresponding potassium concentration, in ppm, from the calibration curve.
D-1.12 Calculation
(1) If the sample solution was made up to 250 ml. in PROCEDURE, step (2) calculate the concentration of
potassium in the sample by the equation.
% K2O = A /2
Where
A is the concentration of potassium, in ppm obtained from the calibration curve, in PROCEDURE, step
(8).
(2) If the sample solution was made up to 500 ml. in PROCEDURE step (2) calculate the concentration by
the equation. K20 == A
D-1.13 Reporting:
Report the result as: Potassium .--------- % K2O (w/v )
Indicate in the report which alternative was used to deter-mine the potassium content by inserting an A in the
parentheses after % K20 for the sodium tetraphenyl boron method or a B for the flame photometric procedure.
SDC/ PSQCA
PS: 5469-2020
APPENDIX 'E'
E-1 MICRO AND SECOUNDARY NUTRIENTS CONTENT
E-1.1 Scope:
The procedure is intended for the determination of trace elements in liquid fertilizers.
E-2 Zn, Fe, Mn, Cu, Ca, Mg determination.
E-2.1 Apparatus:
Poly propylene volumetric flask, 50 ml
Pipette, 2 ml
Weighing balance
Funnel with stand
Wash bottle
Water bath
Burner
Beaker, 50 ml
Atomic Absorption Spectrophotometer
E-2.2 Procedure:
1. Take 1 ml sample in 100 ml vol flask and make up volume.

2. Make dilutions as per calibration standards
3. Run appropriate standards on AAS
4. Run sample
5. Read on concentration mode by atomic absorption spectrophotometer.
E-2.3 Chelated Minerals:
Take 5 ml of liquid sample in 250 ml flask. Make volume with Na2CO3 (0.1M) solution. Non-Chelated
mineral will precipitate, filter the solution through whatman filter paper number 42.
Take 1 ml of filtrate add 5 ml conc. H2SO4 and make volume 100 ml with dis. water. Then proceed as per E-
2.2.
E-2.4 Calculations:
Micronutrients (ppm) = reading x dilution factor
E-3 MICRO NUTRIENTS DETERMINATION
E-3.1 Scope:
The procedure is intended for the determination of trace elements in liquid fertilizers.
E-3.2 Apparatus:
Poly propylene volumetric flask, 50 ml
Pipette, 2 ml
Weighing balance
Funnel with stand
Wash bottle
Water bath
Burner
Beaker, 50 ml
Spectrophotometer.

SDC/ PSQCA
PS: 5469-2020
E-3.3 COLOR DEVELOPMENT (AZOMETHINE – H METHOD)
E-3.3 Reagents:
1. Buffer solution: Dissolve 250 g ammonium acetate and 15 g of ethylenediamine tetra acetic acid (EDTA) in
400 ml of distilled water. Slowly add 125 ml glacial acetic acid and mix.
2. Azomethine – H reagent: Dissolve 0.45 g of reagent in 100 ml of 1 % L-ascorbic acid solution. Fresh
reagent should be prepared and store in a refrigerator.
E-3.3 Calibration Standards
1. Boron standard solution: Dissolve 5.709 g of boric acid (H3BO3) in distilled water (for hot water extraction)
and in 0.05 M HCl for HCl extraction and adjust the volume 1000 ml . This will be of 1000 ppm of boron
solution. Make sub-stock solution to 100 ml of 100 ppm B. Then make working standard as desired.
C1V1 = C2V2
100 x V1 = 0.5 x 100
5 x 100
V1 = ---------- = 0.5 ml of sub-stock solution to make 0.5 ppm B working standard.
1000
Always run blank for accuracy.
E-3.3 Procedure:
Transfer 1 ml aliquot in 50 ml polypropylene volumetric flask, add 2 ml buffer solution, add 2 ml azomethine-
H reagent and mix. After 30 minutes read absorbance at 430 nm by specrophotometer directly at concentration
mode or by graph using standard curve prepared by using standards.
E-3.3 Calculations:
B (ppm) = R x 100*
Where
R = spectrophotometer reading
100* = total dilution factor.

SDC/ PSQCA
PS: 5469-2020
APPENDIX F
SULPHUR TECHNICAL
*18/TC/M/-
(Ref: CIPAC Vol. E, pp 202 – 204)
1. Sampling: Take at least 100 g.

2. Identity test.
3. Sulphur
F-1 SCOPE: The method is applied for all formulations based on Sulphur. If thiosulphate or other Sulphur
compounds are present a correction must be made for them since both free and combine Sulphur is determined.
F-1.1 OUTLINE OF METHOD:

The Sulphur is converted by refluxing with sodium sulphite to sodium thiosulphate. The thiosulphate is then
titrated with standard iodine solution.
F-1.2 REAGENTS
Sodium sulphite crystals: Na2SO3.7H2O
Formaldehyde 35 % solution
Ethanol, 95%
Acetic acid 20% aqueous solution
Iodine standardized solution, c (1/2 I2)=0.1 mol/l, RE 16.1
F-1.3 APPARATUS
Weighting bottle
Conical flasks, 300 ml with ground glass neck
Reflux condenser to fit the end of the condenser should be square cut, not oblique, so that the walls of the flask
are washed down by refluxing mixture.
Measuring cylinder, 50 ml
Measuring cylinder, 25 ml
Volumetric flask, 250 ml
Pipette, 100 ml
Burette, 50 ml
F-2.0 PROCEDURE
(a) Determination. Weight (to the nearest 0.1 mg) sufficient sample (w g) to contain about 0.250 g of
Sulphur, and transfer to conical flask. Wet the sample thoroughly with ethanol (25 ml). Add water (30 to 40 ml)
and sodium sulphite (5 g). Attach the reflux condenser, warm the mixture slowly to dissolve the Sulphur, the
boil for 1 hour shaking the flask from time to time. At the end of this time all the particles of Sulphur ought to
be dissolved. If not, continue heating the mixture. If the element Sulphur is present shake the flask frequently in
order to wash the particles of undissolved Sulphur back into the flask. Cool the solution, remove the condenser,
and transfer quantitatively, to the volumetric flask. Make up to the mark with water, mix thoroughly, filter if
necessary and pipette 100 ml into a conical flask. Add formaldehyde (12.5 ml) and allow the mixture for 5 min.
Add acetic acid (10 ml) and titrate immediately with iodine using starch as indicator.
1 ml iodine, c (1/2 I2) = 0.1 mol/l = 0.032 g Sulphur

SDC/ PSQCA
PS: 5469-2020
(b) Calculation
Sulphur content =8.02 . t / w g/kg

Where
t = ml required for the sample determination
w= mass of sample taken
(c) Correction for thiosulphate. Weight (to the nearest 0.1 mg) sufficient sample (mg) to contain about
0.250 g of Sulphur and transfer to 250 ml conical flask. Add water to suspend the product and sake the mixture
to dissolve the thiosulphate. Make up to the mark, mix thoroughly, and filter or centrifuge the suspension at
3000 rpm for 15 to 30 min. Pipette 100 ml into a 300 ml titration flask, add formaldehyde (12.5 ml) and allow
to stand for 5 min. Add acetic acid (10 ml) and titrate immediately with iodine solution (b ml) using starch as
indicator.
(d) Correction.
Sulphur content from thiosulphate present = 8.02 . b / m g/kg
Where
b = ml required for the thiosulphate determination
m = mass of sample taken (g)
Substrate the content found from that obtained under (b).
*CIPAC method 1967. Prepared by the Sulphur Subcommittee of PAC; Chairman, R de B Ashworth. J Henriet
made a major contribution of the work of the subcommittee.
APPENDIX- G.
INSULUBLE MATTER
G-1 Dissolve 25 ml of the material in 125 ml water and add 1 ml of 10 % diluted Sulphuric Acid. Boil the
solution few minutes. Filter through a weighed and prepared Gooch Crucible Sintered glass crucible
(G.No.4) and wash the residue thoroughly hot water. Dry the crucible at 110 + 5 0C to constant mass.
Then calculate the residue in percent.(Ref PS 4750).
G-2 If the material is in suspension then add the required and relevant acid or compound to react with
nutrient and proceed for above method. In this standard, some nutrients like Sulphur are insoluble in
water so important is to know the inert matter instead of water insolubility.

SDC/ PSQCA

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PS: 5469-2020

PAKISTAN STANDARD SPECIFICATION FOR

LIQUID NUTRIENT SUPPLEMENT

(ALL RIGHTS RESERVED)

Licensed to Company M/s Avan Agro

PAKISTAN STANDARDS SPECIFICATION

Chemical Division P-1/38

4. PACKING AND MARKING:

SAMPLING OF LIQUID FERTILIZERS FROM CONTAINERS AND

A-5 NUMBER OF TESTS:

B-0.1 Detection of Nitrates:

B-1 IMPROVED KJELDAHL METHOD FOR NITROGEN CONTENT OF

B-2 IMPROVED KJELDAHL METHOD FOR NITROGEN CONTENT OF FERTILIZERS CONTAINING

Unless otherwise indicated, the purity of all reagents is intended to be of reagent-grade.

References to water in the following paragraphs mean distilled or deionized water:-

Chemical Division P-7/38

Chemical Division P-8/38

B-3 AMMONICAL NITROGEN IN LIQUID FERTILIZERS

B-3.1 Summary of Method:

(1) Magnesium Oxide (carbonate free)

Chemical Division P-9/38

% Ammoniacal Nitrogen = (A-B)×N×0.0141×100

Ammoniacal Nitrogen----------------------% (Vol.)

B-4.4 AMMONIUM AND NITRATE NITROGEN BY DEVARD’S METHOD

Reference to water in the following paragraphs mean distilled or deionized water.

Chemical Division P-11/38

Report the results to the nearest 0.1 % as total N (Ammoniacal+Nitrate nitrogen).

B-5 BIURET CONTENT OF MIXED FERTILIZERS

B-5.2 Summary of Method:

Calculate the percent of biuret in the sample by the following equation:-

Report the result to the nearest 0.01 % as :

Biuert Content _____________% (vol.)

C.0 PHOSPHORUS CONTENT OF FERTILIZERS:

This section includes the following test procedures:-

C-1 PHOSPHORUS (TOTAL CONTENT OF FERTILIZERS)

Chemical Division P-14/38

C-1.2 Summary of Method:-

Chemical Division P-15/38

C-1.5 Preparation of Sample Solution:

Calculate the phosphorus content (as P205) by the equation.

% (Vol.) P205 = A—B × C × 100

Chemical Division P-17/38

Calibration Concentration, mg. Volume of Standard

C-1.11 Preparation of Sample Solution:

Chemical Division P-18/38

Phosphours, Total (as P205)----------% P205 (vo1.)

Chemical Division P-19/38

C-2 PHOSPHORUS (WATER-SOLUBLE) CONTENT OF FERTILIZERS

C-2.2 Summary of Method:

C-2.3 Preparation of Sample Solution:

Chemical Division P-20/38

C-2.4 A. VOLUMETRIC METHOD:

Chemical Division P-21/38

Calculate the concentration of water-soluble phosphorus in the sample as:

% P205 = (A-B) × V1 × 100

A is the volume of standard alkali solution used to dissolve the precipitate, in ml

(2) Molybdovanadate Solution—Dissolve 40 g. of ammonium molybdate tetrahydrate, (NH4)6 MO7O24

Calibration Solution Concentration Volumes of Standard

Chemical Division P-23/38

S is the weight of sample taken for analysis, in g.