Title of Invention	SIMPLIFIED INDUSTIVELY COUPLED PLASMA SPECTROMETRIC METHOD FOR ESTIMATION OF FE(MET) IN SPONGE IRON
Abstract	1. A simplified ICP Spectrometric method for estimation of Fe(met) in sponge iron in a sample comprising the step of: - taking 0.1-0.5 gm sample in a clean and dried volumetric flask; - adding 60-70 ml boiled filter water and 1.0-2.0 gm mercuric chloride to the volumetric flask containing the sample to convert metallic iron to ferrous chloride; - cooling the flask ; - filtering the contents of the flask ; - collecting the filtrate into a volumetric flask; - washing the residue with boiled filter water at least five times, adding the washings to the filtrate and making up the volume of the filtrate up to 100 ml; - calibrating the ICP spectrometer using four synthetic standards having concentration 0,100,500 and 800 ppm; - matching the matrix of calibration standards with sample solution by adding same quantity of mercuric chloride; - making the measurement in ICP using 259.44 nm spectra line.

Title of Invention

SIMPLIFIED INDUSTIVELY COUPLED PLASMA SPECTROMETRIC METHOD FOR ESTIMATION OF FE(MET) IN SPONGE IRON

Abstract

1. A simplified ICP Spectrometric method for estimation of Fe(met) in sponge iron in a sample comprising the step of: - taking 0.1-0.5 gm sample in a clean and dried volumetric flask; - adding 60-70 ml boiled filter water and 1.0-2.0 gm mercuric chloride to the volumetric flask containing the sample to convert metallic iron to ferrous chloride; - cooling the flask ; - filtering the contents of the flask ; - collecting the filtrate into a volumetric flask; - washing the residue with boiled filter water at least five times, adding the washings to the filtrate and making up the volume of the filtrate up to 100 ml; - calibrating the ICP spectrometer using four synthetic standards having concentration 0,100,500 and 800 ppm; - matching the matrix of calibration standards with sample solution by adding same quantity of mercuric chloride; - making the measurement in ICP using 259.44 nm spectra line.

Full Text	FIELD OF INVENTION The present invention relates to a Simplified Inductively Coupled Plasma (ICP) Spectrometrc method for estimation of Fe (met) in sponge iron. BACKGROUND OF THE INVENTION The process of sponge iron making aims to remove oxygen from iron ore, wherein the departing oxygen causes micro pores in the ore body making it porous. The quality of sponge iron is primarily ascertained by the percentage of metallization (removal of oxygen), which is the ratio of metallic iron to the total iron present in the product. Hence estimation of Fe(met) accurately is of prime importance to ascertain its quality. There are two methods which are commonly used for estimation of Fe(met). One is the Ferric Chloride method and the other is the bromine methanol method. In the ferric chloride method, to about 1.0 gm of the sample 200 ml of FeCI3 solution is added and the mixture stirred for one hour. The mixture is then filtered and to the filtrate 400 ml of water, 25 ml of HCI, 25 ml of H3PO4 and 3-4 drops of diphenyl amine sulfonate is added. The resulting solution is titrated with 0.1N K2Cr2O7. In the bromine methanol method, the combined iron and total iron are estimated separately and the difference between the two is taken as the metallic iron. OBJECTS OF THE INVENTION It is therefore, an object of the present invention to propose an ICP Spectrometrc method for estimation of Fe(met) which is an easier method than the existing state of Arts. Another object of the present invention is to propose an ICP Spectrometrc method for estimation of Fe(met) which is faster and less time consuming. A further object of the present invention is to propose an ICP Spectrometrc method for estimation of Fe(met) which consumes less number of chemicals. BRIEF DESCRIPTION OF THE INVENTION In a 500 ml conical flask distilled water is filled half and boiled to remove dissolved oxygen. Then 0.1-0.5 gm sample is taken in a clean and dried 100 ml volumetric flask. 60-70 ml of oxygen free water is added and 1.0-2.0 gm mercuric chloride is added to the flask to convert metallic iron to ferrous chloride. Fe + HgCI2 = FeCI2 + Hg The flask is then cooled by covering the mouth of the flask. The contents are then filtered through grade 41 filter paper and filtrate collected into a 100 ml volumetric flask. The residue is washed five times with oxygen free water and then the volume is made up to 100 ml. The ICP Spectrometer is calibrated using four synthetic standards having iron concentration of 0, 100, 500 and 800 ppm. The calibration standards are matrix matched with the sample solution by adding the same quantity of mercuric chloride. 259.44 nm line is used for making the measurements in ICP. The method can also be used for determination of metallic iron content in iron and steel making slag and other related materials. If the metallic Fe content is less than 10% then 0.5g of the sample is used. To validate the above method, samples have been tested by all the three methods and the results obtained are given below: The close agreement between the results indicate that the method is well capable of estimating Fe(met) content in Sponge Iron. WE CLAIM 1. A simplified ICP Spectrometric method for estimation of Fe(met) in sponge iron in a sample comprising the step of: - taking 0.1-0.5 gm sample in a clean and dried volumetric flask; - adding 60-70 ml boiled filter water and 1.0-2.0 gm mercuric chloride to the volumetric flask containing the sample to convert metallic iron to ferrous chloride; - cooling the flask ; - filtering the contents of the flask ; - collecting the filtrate into a volumetric flask; - washing the residue with boiled filter water at least five times, adding the washings to the filtrate and making up the volume of the filtrate up to 100 ml; - calibrating the ICP spectrometer using four synthetic standards having concentration 0,100,500 and 800 ppm; - matching the matrix of calibration standards with sample solution by adding same quantity of mercuric chloride; - making the measurement in ICP using 259.44 nm spectra line. 2. An ICP Spectrometric method for estimation of Fe(met) as claimed in claim 1 which can also be used for estimation of Fe(met) in iron and steel making slags. 1. A simplified ICP Spectrometric method for estimation of Fe(met) in sponge iron in a sample comprising the step of: - taking 0.1-0.5 gm sample in a clean and dried volumetric flask; - adding 60-70 ml boiled filter water and 1.0-2.0 gm mercuric chloride to the volumetric flask containing the sample to convert metallic iron to ferrous chloride; - cooling the flask ; - filtering the contents of the flask ; - collecting the filtrate into a volumetric flask; - washing the residue with boiled filter water at least five times, adding the washings to the filtrate and making up the volume of the filtrate up to 100 ml; - calibrating the ICP spectrometer using four synthetic standards having concentration 0,100,500 and 800 ppm; - matching the matrix of calibration standards with sample solution by adding same quantity of mercuric chloride; - making the measurement in ICP using 259.44 nm spectra line.

Full Text

FIELD OF INVENTION
The present invention relates to a Simplified Inductively Coupled Plasma (ICP) Spectrometrc method for estimation of Fe (met) in sponge iron.
BACKGROUND OF THE INVENTION
The process of sponge iron making aims to remove oxygen from iron ore, wherein the departing oxygen causes micro pores in the ore body making it porous.
The quality of sponge iron is primarily ascertained by the percentage of metallization (removal of oxygen), which is the ratio of metallic iron to the total iron present in the product. Hence estimation of Fe(met) accurately is of prime importance to ascertain its quality.
There are two methods which are commonly used for estimation of Fe(met). One is the Ferric Chloride method and the other is the bromine methanol method.

In the ferric chloride method, to about 1.0 gm of the sample 200 ml of FeCI3 solution is added and the mixture stirred for one hour. The mixture is then filtered and to the filtrate 400 ml of water, 25 ml of HCI, 25 ml of H3PO4 and 3-4 drops of diphenyl amine sulfonate is added. The resulting solution is titrated with 0.1N K2Cr2O7.
In the bromine methanol method, the combined iron and total iron are estimated separately and the difference between the two is taken as the metallic iron.
OBJECTS OF THE INVENTION
It is therefore, an object of the present invention to propose an ICP Spectrometrc method for estimation of Fe(met) which is an easier method than the existing state of Arts.
Another object of the present invention is to propose an ICP Spectrometrc method for estimation of Fe(met) which is faster and less time consuming.
A further object of the present invention is to propose an ICP Spectrometrc method for estimation of Fe(met) which consumes less number of chemicals.

BRIEF DESCRIPTION OF THE INVENTION
In a 500 ml conical flask distilled water is filled half and boiled to remove dissolved oxygen. Then 0.1-0.5 gm sample is taken in a clean and dried 100 ml volumetric flask.
60-70 ml of oxygen free water is added and 1.0-2.0 gm mercuric chloride is added to the flask to convert metallic iron to ferrous chloride. Fe + HgCI2 = FeCI2 + Hg
The flask is then cooled by covering the mouth of the flask. The contents are then filtered through grade 41 filter paper and filtrate collected into a 100 ml volumetric flask. The residue is washed five times with oxygen free water and then the volume is made up to 100 ml. The ICP Spectrometer is calibrated using four synthetic standards having iron concentration of 0, 100, 500 and 800 ppm. The calibration standards are matrix matched with the sample solution by adding the same quantity of mercuric chloride. 259.44 nm line is used for making the measurements in ICP.

The method can also be used for determination of metallic iron content in iron and steel making slag and other related materials. If the metallic Fe content is less than 10% then 0.5g of the sample is used.
To validate the above method, samples have been tested by all the three methods and the results obtained are given below:

The close agreement between the results indicate that the method is well capable of estimating Fe(met) content in Sponge Iron.

WE CLAIM
1. A simplified ICP Spectrometric method for estimation of Fe(met) in sponge iron in a sample comprising the step of:
- taking 0.1-0.5 gm sample in a clean and dried volumetric flask;
- adding 60-70 ml boiled filter water and 1.0-2.0 gm mercuric chloride to the volumetric flask containing the sample to convert metallic iron to ferrous chloride;
- cooling the flask ;
- filtering the contents of the flask ;
- collecting the filtrate into a volumetric flask;
- washing the residue with boiled filter water at least five times, adding the washings to the filtrate and making up the volume of the filtrate up to 100 ml;
- calibrating the ICP spectrometer using four synthetic standards having concentration 0,100,500 and 800 ppm;
- matching the matrix of calibration standards with sample solution by adding same quantity of mercuric chloride;
- making the measurement in ICP using 259.44 nm spectra line.

2. An ICP Spectrometric method for estimation of Fe(met) as claimed in claim 1 which can also be used for estimation of Fe(met) in iron and steel making slags.

1. A simplified ICP Spectrometric method for estimation of Fe(met) in sponge iron in a sample comprising the step of:
- taking 0.1-0.5 gm sample in a clean and dried volumetric flask;
- adding 60-70 ml boiled filter water and 1.0-2.0 gm mercuric chloride to the volumetric flask containing the sample to convert metallic iron to ferrous chloride;
- cooling the flask ;
- filtering the contents of the flask ;
- collecting the filtrate into a volumetric flask;
- washing the residue with boiled filter water at least five times, adding the washings to the filtrate and making up the volume of the filtrate up to 100 ml;
- calibrating the ICP spectrometer using four synthetic standards having concentration 0,100,500 and 800 ppm;
- matching the matrix of calibration standards with sample solution by adding same quantity of mercuric chloride;
- making the measurement in ICP using 259.44 nm spectra line.

Documents:

http://ipindiaonline.gov.in/patentsearch/GrantedSearch/viewdoc.aspx?id=OrS41x2OoCQ40dcbNlvVeQ==&loc=wDBSZCsAt7zoiVrqcFJsRw==

« Previous Patent

Next Patent »

Patent Number

270363

Indian Patent Application Number

144/KOL/2009

PG Journal Number

51/2015

Publication Date

18-Dec-2015

Grant Date

16-Dec-2015

Date of Filing

27-Jan-2009

Name of Patentee

TATA STEEL LIMITED

Applicant Address

RESEARCH AND DEVELOPMENT AND SCIENTIFIC SERVICES DIVISION, JAMSHEDPUR

Inventors:

#	Inventor's Name	Inventor's Address
1	MR. K N UDPA	TATA STEEL LIMITED, JAMSHEDPUR 831 001
2	MR.SUBRATA PATRA	TATA STEEL LIMITED, JAMSHEDPUR 831 001

PCT International Classification Number

G01C 19/64

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA