Metallurgical Analysis.
Phosphorus Determination Method.
Determination Of Phosphorus in Silico Manganese, Ferro Manganese and its ores etc.
Economically feasible and effective determination of phosphorus by the volumetric (alkalimetric) method of chemical analysis in minimum time.
......by Sp Shende and Balaji Group India
We are metallurgical analyst having more than 15 years experience. We do daily analysis of Mn, Si, Fe, MnO, SiO2, Al2O3, CaO, MgO, P, C, S and coke, coals FC 's etc. It's our daily work in our Laboratory. Out of this, we now see the "Method of determination of Phosphorus" i.e. "How to find out Phosphorus ? " in Silico manganese, Ferro manganese metals and it's ores etc.
We always find out Phosphorus through this procedure daily in our Laboratory. With using this method, you can find out Phosphorus within four hours approx. Several metallurgical chemist comes in our laboratory and learn, applied and compared to standard Lab Samples results in their labs. And agreed that, It's a perfect method to find out phosphorus in minimum time !
After applying this method, your search for 'How to Find out Phosphorus' ends here !
Let we explain this genuine research and experienced method for Determination of Phosphorus step by step here. Let's Start now !
01. As per your requirement, Take crushed and 100 mesh fine powder of Silico manganese or Ferro manganese or Ore sample. And dry this sample in oven at 105 degree centigrade for one hour. And keep it aside to attain a room temperature (27 – 30 degree centigrade). Weight out 0.5gm or 01 gm of sample for your analysis.
02. Baking Process :-
Depending on your samples, You may use : Either A. Baking using HF for finding out low phosphorus (LP – 0.5 to 0.15%)samples, OR B. Baking using Aquargia for finding out high phosphorus (HP)samples, in your baking process . Choice is yours !
Either :
A. Baking using HF :- Take 0.5gm or 01gm oven dried moisture free sample of metal or ore, in 500 ml-Teflon or glass beaker. And add 35 ml Concentrated Nitric Acid (HNO3) in it. Place it on hot plate. After warm, add drop by drop Concentrated Hydrofluoric (HF) acid in it, until the vigorous reaction has subsided. (it takes 5 ml HF approx.). Remain it on hot plate.
Note :- Some chemist group don’t prefer this baking using HF for phosphorus formation. Because free sulphate and fluoride ions are totally objectionable. However, a little fluoride is tolerable when the phosphorus. precipitation is carried out in presence of boric acid. Hence seller side chemist prefer it for avoiding dispute between seller and buyer.
OR :
B. Baking using Aquargia( HCL : HNO3 | 03 : 01 ) :- Take 0.5gm or 01gm oven dried moisture free sample of metal or ore, in 500ml-glass beaker. : Add 30 ml Concentrated Hydrochloric Acid (HCL) in it, And then add 10ml concentrated Nitric Acid (HNO3) in it. Place it on hot plate.
Place it on hot plate : Either A. or B. solution. And evaporate it slowly up to entirely dryness. After dryness : Further remains it on hot plate for approx. 20
for baking. This is call as baking process. This baking process takes approx. 60 minutes
03. Re baking :- Add approx. 20 ml Concentrated HCL in above beaker’s baked mass. Then again it evaporate slowly over a hot plate up to completely dryness. After dryness further bake it for approx. 10 minutes on hot plate.
04. Re dissolvetion :- After completed baking, take out baked and completely dried mass containing beaker, from hot plate. And cool it for five minutes at room temperature (27-30 degree C).
After 5 Minutes cooling, now add 40ml Concentrated Hydrochloric (HCL) in that residue, and again place it on hot plate until the HCL quantity becomes Half (i.e. up to 20ml).
After half quantity reduction of Concentrated HCL, now add approx. 20ml distilled water in it, so that the quantity become again aprrox. 40ml in beaker. And again remains it on hot plate until the quantity becomes again half ( i.e. approx. 20ml).
This approx. 20 to 15ml solution is your pasty mass residue solution. This redissolved pasty mass residue solution making process, is called as Redissolvetion process. This redissolvetion process takes approx. 40 to 50 minutes.
Remember that : Hydrochloric(HCL) acid concentration up to 15% at the time of phosphorus precipitation in terms of free chloride ion is tolerable.
05. Filtration :- Take out beaker containing redissolved pasty mass residue solution, from hot plate. And add approx. 15 to 20ml distilled water in it. Warm it. And filter this warm solution through 1 No. Whatman's filter paper. Wash filter paper 2-3 times with warm distilled water. After finishing washing, throw out filter paper having Si- Ppt. Only take filtrate solution in conical flask. Make up it up to approx. 100 ml, by adding distilled water in it. Take it for further analysis.
06. Add approx. 05 to 07ml Concentrated Nitric acid in above filtrate solution. And then boil it. After boiling, keep it aside to attain approx. 90 to 80 degree centigrade temperature.
Take this flask containing filtrate solution of approx. 90 to 80 degree centigrade and shake it. While continuously shaking : Count and add drop by drop potassium permanganate [KMnO4 (2% )] solution in it, till the color changes occurs(say 05 drops).
After KMnO4 color persist, now count and add drop by drop Sodium Nitrate [NaNO3 (2%)] solution until the color becomes toward original color yellow (say 05 drops).
If more than sufficient amount of KMNO4 drops is added, then it may forms Manganese oxide precipitate(Ppt.). If such Ppt. appears in above, then boil it and destroy this excess KMNO4 color ppt. with further adding 2 to 4 drops of 2% Sodium Nitrate(NaNO3 ) solution. Or this KMNO4 color Ppt. is bleached by adding 2% Sodium Sulphate or Hydrogen peroxide in just sufficient quantity.
After approx. original yellow color formation, now dilute it by adding some distilled water say 25ml. Then visually inspect it : If some precipitate still appears in it, then Filter it. And take filtrate in 500-ml conical flask for further analysis.
07. Take above 500-ml conical flask solution : If you have used step 02 -A. baking with HF line, then add 02 gm boric acid to the flask solution and heat it up to completely dissolve. Else for step 02-Baking with aqua line, only boil it.
Keep boil solution aside to attain a 60 degree centigrade temperature.
And at approx. 60 degree centigrade, neutralize it as :
I. Add Concentrated Ammonia Solution slowly in it until the black precipitate forms.
II. After black precipitate formed by ammonia, now add Concentrated Nitric acid (HNO3) slowly in it until the black precipitate completely disappeared.
After disappearing precipitate : add excess approx. 04 to 07ml Concentrated Nitric acid in it.
Remember that : while adding excess nitric acid, the concentration of nitric acid at the time of phosphorus precipitation should not exceed 07% by volume.
08. Phosphorus precipitation formation :- Make the volume of above solution up to approx. 150 to 200 ml and then Boil it.
If you have used step 02-B. baking with Aqua line, then add 10 ml of 10%Ammonium Nitrate(it’s optional). And boil it. Remember that : Addition of more ammonium nitrate than what is present in the reagent itself is superfluous.
Else for HF baking line : only Shake and keep it aside to attain approx 90 degree centigrade temperature .
At approx. 90 to 80 degree centigrade, now add 50 ml freshly filtered Ammonium Molybdate solution. And shake vigorously for 20 minutes or up to sufficient yellow precipitate(Ppt.) formations occurs i.e. color become yellow indicates that, the Ammonium phospho-molybdate precipitate formation is done. It takes aprox.15min.to 25 min
Keep in mind that : Temperature of solution in flask before addition of molybdate solution should be initially kept between 80 to 90 degree centigrade, so that after adding molybdate solution, it’s temperature down to 70 degree centigrade. At 70 to 65 degree centigrade, ammonium phospho-molybdate precipitated. Hence remember that : while vigorously continuous shaking flasks, the temperature of solution in flask remains between 80 to 70 degree centigrade. It should not down to 65 degree centigrade.
Now For Settle down this formed Ammonium phospho-molybdate precipitate at the bottom of flask : Either keep it warm at 60 degree centigrade for 30 to 45 minutes, Or place this flask on hot top of the Muffle furnace for 30 to 45 Minutes.
09. Filtration :- After Settlement of yellow precipitated phosphorus at the bottom of flask, now take it for filtration process. Filter this yellow precipitated phosphorus by using 41 No.(125mm
Care should be taken that : Filter paper must not dried during filtering process. Hence continuously filter it without break. If you break filter process and filter paper dried by air, then dried and free phosphorus on filter paper may react with air, and thus it may affects your analysis results.
After passing out last drop through funnel : Transfer remaining yellow precipitate in conical flask onto the funnel 's filter paper. For transferring remaining yellow precipitate in to conical flask on funnel's filter paper : Don't use distilled water because phosphorus may dissolved in distilled water. Instate of distilled water, use cold 1% Nitric acid wash solution for transferring yellow precipitated phosphorus from flask to funnel's filter paper. After completely transfer of yellow precipitated phosphorus on filter paper : Now you may acidify collected phosphorus on filter paper, by further pouring approx.10 ml cold 1% Nitric acid [HNo3(1%)] wash solution on it.
After passing out last drop of 1% Nitric acid [HNo3(1%)] wash solution through funnel : Now make this phosphorus acid free by washing it 3 to 4 times with 01% Potassium Nitrate [KNO3(1%)] wash Solution, until the yellow phosphorus on filter paper become acid free.
10. To check acid freeness :- Take last 10 drops of 1% KNO3 wash solution’s each addition, from Funnel : Then add 01 drop Phenolphthalein Indicator in it. And then add 01 drop of NaOH(0.1N) in it. And observed that : IF color become pink by adding single drop of NaOH (0.1N ) , then yellow precipitated phosphorus on filter paper is Acid free.
If color does not appears pink by adding single drop of NaOH , then further washing required. Further wash yellow precipitated phosphorus on filter paper by pouring 01% Potassium Nitrate [ KNO3(1%) ] wash Solution up to yellow precipitated phosphorus on filter paper completely become acid free. It is done by repeatedly checking above acid free test.
Remember that : Washing solution of Potassium Nitrate [KNO3(1%)] must not to much exceed. Hence after each addition of 1% KNO3 solution in funnel, you must have to check repeatedly acid free test.
11. Titration :- Transfer this Acid free yellow precipitated phosphorus containing Filter paper : To the well washed original Conical flask, where the phosphorus was first precipitated. Now you may add desired quantity of distilled water in that flask, to dissolved yellow phosphorus. Now titrate it as follows
Add N/10 Sodium hydroxide [ NaOH (0.1N) ] solution in it up to the colorless/white color forms ( Called it as Blank Taken. or say 25ml as blank taken ). Shake it well and then add drops of Phenolphthalein Indicator in it.
After adding drops of Phenolphthalein indicator : Colorless solution became to pink color solution.
Now titrate this pink color solution with N/10 Hydrochloric acid [ HCL(0.1N ) ] solution up to completely Colorless endpoint. i.e. pink color completely disappears and it becomes original colorless solution. At this original colorless/white color point, Take Burette Reading (Say BR)
12. Phosphorus Formulas :-
% P = [ (Blank Taken - BR) x 0.001354 x N x 100 ] ÷ weight of Sample Taken
± standard Difference error
where
% P = Phosphorus percentage%
Blank Taken = NaOH (0.1N) solution ml-quantity taken in flask up to the colorless/white color forms.
BR = Burette Readings : End point reading of titration.
N = Normality 0.1 N of NaOH & HCl solutions. (NaOH and HCL Both solution must have same normality)
± Standard Difference error :-
By the above procedure : Find out phosphorus of Standard Sample and its difference.
For example : Suppose Standard sample’s Known phosphorus is 0.04. And by above procedure : If that standard sample phosphorus result comes as 0.06, than standard difference is 0.06-0.04 = 0.02 , is subtracted as standard difference error in your above procedure result.
Remember that : Whenever you makes any new solutions required for this procedures, you must find out first Standard difference using Standard Sample.
Note :- Always use pure distilled water in this procedures as well as in solution makings procedures. Care should be taken that : Not a single drop of Tab water remains in your glassware. Hence wash glassware by distilled water firstly.
Chemicals Required for Phosphorus Procedures : -
01. Nitric acid ( HNO3) min 69% GR grade : Merck or equivalent.
02. Hydrochloric acid (HCL ) ) min 35% GR grade : Merck or equivalent.
03. Hydrofluoric acid (HF ) about 40% HF GR grade : Merck or equivalent.
04. Ammonia Solution ( NH3 ) min 25% GR grade : Merck or equivalent.
05. Potassium per Manganate ( KMnO4 ) GR grade : Merck or equivalent.
06. Potassium Nitrate purified (KNO3 ) GR grade : Merck or equivalent.
07. Sodium nitrate purified ( NaNO3 ) : Merck or equivalent.
08. Sodium hydroxide ( NaOH =40.00 ) : Merck or equivalent.
09. Phenolphthalein Indicator PH 8.2 - 9.8 : Merck or equivalent.
10. Ammonium Nitro Molybdate GR grade : Merck or equivalent .
OR Ammonium heptamolybdate tetra hydrate pure : Merck Or equivalent.
11. Silver Nitrate (AgNO3) crystals : Merck or equivalent.
12. Methyl orange : Merck or equivalent.
13. Ammonium Nitrate pure. Merk or equivalent.
14. Boric Acid - pure powder. Merck or equivalent.
15. Whatman filter paper ashless No.41. ( 125mm φ x 100 circles : Cat. No. 1441-125 )
Whatman filter paper qualitative No.1. ( 125mm φ x 100 circles: Cat. No. 1001-125 )
Solutions preparation for phosphorus procedure :-
Remember that : While making any solutions, only use pure distilled water. Don't use tab water, because tab water itself contains small amount of phosphorus, chlorine etc. salts, which affects your results.
How to check pure distilled water ?
Care should be taken that : Not a single drop of Tap water remains in your glassware. Hence wash 500ml-beaker by distilled water one or two times. And then take 100ml distill water in that washed beaker. And add 0.5gm silver Nitrate crystals in it. And observe that : If white precipitate is not form, then it is pure distilled water. If milky white precipitate formed, then that water is not a pure distilled water.
Solutions preparation :-
01. Potassium permanganate [ KMnO4 (2% ) ] solution:-
Take 100ml distilled water : And add 02 gm KMnO4 crystals in it.
Shake and dissolved it well. Pour it in dropper. Label it. And store it at cool place.
02. Sodium Nitrate [ NaNO3 (2%) ] solution :-
Take 100ml distilled water : And add 02 gm NaNo3 power in it.
Shake and dissolved it well. Pour it in dropper. Label it. And store it at cool place.
03. Ammonium Molybdate solution :-
Take two Conical flask : say 01 lit-flask A & 02 lit-flask B.
Well wash it by distilled water.
A. Take 100ml Concentrated Ammonia Solution in conical flask A :
And add 60gm Ammonium Molybdate powder in it.
Stirred well up to molybdate powder dissolved in it.
Then again : Add 50ml distilled water in it. And again stirred well.
Once more again : Add 50ml distilled water in it. And stirred it up to completely dissolved Molybdate powder.
Thus in A Flask : you have taken 100 ml Concentrated Ammonia Solution.
+ 60 gm Molybdate powder + 100ml distilled water. Cool it well.
B. Take 300 ml distilled water in 2-litre capacity conical flask B. And add 250 ml Concentrated Nitric acid (HNO3) slowly in it, with continuous shaking and cooling flask. After completely adding of HNO3, further Cool it and keep it aside separately.
After cooling both A and B flask solutions : Now add A flask solution slowly, in to B flask Solution with continuous shaking and cooling. i.e. Mixed it by adding solution A. in Solution B. This mixed solutions is your final Ammonium Molybdate solutions. Allow it for settlement. After giving sufficient settlement time to this solution, Observed it that : If some yellow precipitate appears, then Filter it by No. 1 Whatman's filter paper. And then Store it at cool place.
Remember that : Whenever you adds acid into water, heat is generated. While adding acid into water : If flask become hot, then stop the adding of HNO3 and cool the flask first and again start adding of HNO3.
04. Nitric acid [ HNO3(1%) ] wash solution :-
Take 1000ml distilled water : And add 10ml Concentrated HNO3 in it slowly.
Shake and mixed it.
05. Potassium Nitrate [ KNO3(1%) ] wash Solution :-
Take 1000ml distilled water ; And add 10gm KNO3 powder in it.
Shake and dissolved it.
06. Sodium hydroxide N/10 [ NaOH (0.1N) ] solution :-
Take 1000ml distilled water and add 04 gm NaOH pallets in it.
Shake and dissolved it.
07. Hydrochloric acid N/10 [ HCL (0.1N ) ] solution:-
Take 1000ml distilled water. And add 8.28 ml concentrated HCL in it.
shake and mixed it.
OR
Nitric acid N/10 [ HNO3 ( 0.1N ) ] :-
Take 1000ml distilled water. And add 6.26 ml concentrated HNO3 in it. shake and mixed it. And Standardize it against standard sodium carbonate solution, using methyl orange as indicator.
Balancing of NaOH ( 0.1N ) and HCL ( 0.1N ) solutions :-
Take 10 ml NaOH (0.1N) solution. And add 1 or 2 drops of phenolphthalein
indicator in it. And titrate it with HCL ( 0.1N ) solutions up to the colorless endpoint.
If your Burette Reading is 10, then these two solutions are perfectly balanced, Else balance it by adding drops of distilled water in one of solutions.
OR find out error as : Error = 10/BR. And multiply this Error to your final result.
08. Phenolphthalein Indicator :-
Take 100 ml Methanol. And add 05 gm Phenolphthalein indicator powder in it.
Shake and dissolved it. Pour it in dropper. Label it. And store it at cool place.
OR
Dissolve 01 gm Phenolphthalein powder in 100 ml of alcohol.
And dilute with 100 ml of distilled water with constant stirring.
09. Methyl Orange Indicator :-
Dissolve 01 gm methyl orange powder in 100 ml distilled water. Pour it in dropper.
Label it. And store it at cool place.
10. Ammonium Nitrate 10 % solutions :-
Take 100ml distilled water. And add 10gm Ammonium Nitrate powder in it shake and dissolved it well.
Keywords :-
Metallurgical analysis methods by Sp Shende.
Metallurgical Analysis.
Metallurgical Analysis by Sp Shende.
Phosphorus Determination Method.
Determination Of Phosphorus.
Analysis of phosphorus.
Determination Of Phosphorus by Sp Shende.
Determination Of Phosphorus in Silico Manganese.
Determination Of Phosphorus in Ferro Manganese.
Determination Of Phosphorus in Manganese ores.
Determination of phosphorus by the volumetric (alkali metric) method.
Economically feasible and effective determination of phosphorus.
Method of chemical analysis of phosphorus.
Method of chemical analysis of phosphorus in minimum time.
Method of determination of Phosphorus.
Phosphorus finding procedures.
How to find out Phosphorus ?
How to find out Phosphorus within four hours ?
How to find out phosphorus in minimum time ?
How to check pure distilled water ?
How to check acid freeness of phosphorus ?
How to make Phenolphthalein Indicator ?
How to make Methyl orange Indicator ?
How to prepared molybdate solution ?
Chemicals required for phosphorus.
Solutions for phosphorus.
Analysis of Mn, Si, Fe, MnO, SiO2, Al2O3, CaO, MgO, P, C, S
Finding out Fixed Carbon FC's of pearl coke, steam coals, Charcoals and its analysis.
Sp Shende , S. P. Shende , spshende , sp_shende, Sudan Prabhakar Shende.
Analysis Method contents written by :- Sp Shende.
Emails :-
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Address :- Sp Shende. 64, Om Colony, ArniRoad, Yavatmal 445001 (M.S.) India.
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Paypal email :- spshende@hotmail.com
Links of Other Metallurgical method’s contents may be submitted by Sp Shende :-
Metallurgical Analysis by Sp Shende.
Determination of Manganese (Mn).
Determination of Silica (Si).
Determination of Iron (Fe).
Determination of Phosphorus (P).
Determination of Sulphur (S).
Determination of Carbon (C).
Determination of Manganese dioxide ( MnO2)
Determination of Silica dioxide (SiO2).
Determination of Alumina (Al2O3).
Determination of CaO.
Determination of MgO.
Calculation of Basicity of Furnace.
Determination of Fixed Carbon’s (FC’S) of pearl coke.
Determination of Fixed Carbon’s (FC’S) of Steam Coal.
Determination of Fixed Carbon’s (FC’S) of Charcoals.
How to check PPM of water ?.
Thanks.
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