ASTM E278-01(2015)e1

Standard Test Method for Determination of Phosphorus in Iron Ores by Phosphomolybdate Coprecipitation and Nitric Acid Titrimetry

SIGNIFICANCE AND USE
5.1 This test method is intended to be used for compliance with compositional specifications for phosphorus content. It is assumed that all who use these procedures will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expected that work will be performed in a properly equipped laboratory and that proper waste disposal procedures will be followed. Appropriate quality control practices shall be followed, such as those described in Guide E882.
SCOPE
1.1 This test method covers the determination of phosphorus in iron ores, concentrates, and agglomerates.  
1.2 This test method covers the determination of phosphorus in the range from 0.01 % to 1.00 %.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 14-Nov-2015
• ICS: 73.060.10 - Iron ores
• Technical Committee: E01 - Analytical Chemistry for Metals, Ores, and Related Materials
• Drafting Committee: E01.02 - Ores, Concentrates, and Related Metallurgical Materials

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
´1
Designation: E278 − 01 (Reapproved 2015)
Standard Test Method for
Determination of Phosphorus in Iron Ores by
Phosphomolybdate Coprecipitation and Nitric Acid
Titrimetry
This standard is issued under the fixed designation E278; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Editorial corrections were made in 1.2 and Table 1.
1. Scope E882 Guide for Accountability and Quality Control in the
Chemical Analysis Laboratory
1.1 This test method covers the determination of phospho-
rus in iron ores, concentrates, and agglomerates.
3. Terminology
1.2 This test method covers the determination of phospho-
3.1 Definitions—For definitions of terms used in this test
rus in the range from 0.01 % to 1.00 %.
method, refer to Terminology E135.
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
4. Summary of Test Method
standard.
4.1 The sample is dissolved in HCl and HNO . After the
1.4 This standard does not purport to address all of the
addition of HClO , the solution is evaporated to strong fumes
safety concerns, if any, associated with its use. It is the
to dehydrate the silica. The insoluble residue is filtered off,
responsibility of the user of this standard to establish appro-
ignited, and treated for the recovery of any contained phos-
priate safety and health practices and determine the applica-
phorus. Ammonium molybdate is added to precipitate phos-
bility of regulatory limitations prior to use.
phomolybdate. The precipitate is filtered off and washed free
from acid. It is then dissolved in an excess of standard sodium
2. Referenced Documents
hydroxide solution. The excess sodium hydroxide is titrated
2.1 ASTM Standards:
with a standard solution of HNO using phenolphthalein as an
D1193 Specification for Reagent Water indicator.
E50 Practices for Apparatus, Reagents, and Safety Consid-
erations for Chemical Analysis of Metals, Ores, and 5. Significance and Use
Related Materials
5.1 This test method is intended to be used for compliance
E135 Terminology Relating to Analytical Chemistry for
with compositional specifications for phosphorus content. It is
Metals, Ores, and Related Materials
assumed that all who use these procedures will be trained
E691 Practice for Conducting an Interlaboratory Study to
analysts capable of performing common laboratory procedures
Determine the Precision of a Test Method
skillfully and safely. It is expected that work will be performed
E877 Practice for Sampling and Sample Preparation of Iron
in a properly equipped laboratory and that proper waste
Ores and Related Materials for Determination of Chemi-
disposal procedures will be followed. Appropriate quality
cal Composition and Physical Properties
control practices shall be followed, such as those described in
Guide E882.
This test method is under the jurisdiction of ASTM Committee E01 on
6. Interferences
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
6.1 Vanadium and arsenic, elements commonly found in
responsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-
lurgical Materials.
iron ores, coprecipitate with the phosphorus. Provisions for
Current edition approved Nov. 15, 2015. Published December 2015. Originally
their removal or elimination of their interference are included
ɛ1
approved in 1965. Last previous edition approved in 2010 as E278 – 01 (2010) .
in this test method.
DOI: 10.1520/E0278-01R15E01.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
6.2 Titanium tends to form an insoluble compound with
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
phosphorus and thus may cause low values for phosphorus.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. Provision for its removal is included in this test method.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
E278 − 01 (Reapproved 2015)
7. Reagents and Materials 7.14 Potassium Nitrate, Wash Solution (10 g⁄L)—Dissolve
10 g of potassium nitrate (KNO ) in water, dilute to 1 L, and
7.1 Purity of Reagents—Reagent grade chemicals shall be
mix.
used in all tests. Unless otherwise indicated, it is intended that
all reagents conform to the specifications of the Committee on 7.15 Potassium Permanganate Solution (25 g⁄L)—Dis-
Analytical Reagents of the American Chemical Society where solve 25 g of potassium permanganate (KMnO ) in water and
such specifications are available. Other grades may be used, dilute to 1 L.
provided it is first ascertained that the reagent is of sufficient
7.16 Sodium Carbonate (Na CO ).
2 3
high purity to permit its use without lessening the accuracy of
7.17 Sodium Hydroxide, Stock Solution—Dissolve 300 g of
the determination.
NaOHin1 Lofwater.Addaslightexcessofbariumhydroxide
7.2 Purity of Water—Unless otherwise indicated, references
(Ba(OH) ) to precipitate any carbon dioxide (CO ).Allow any
2 2
to water shall be understood to mean reagent water as defined
precipitate to settle out. Store the solution in a polyethylene
by Type II of Specification D1193.
container.
7.3 Ammonium Molybdate Solution (Acidic).
7.18 Sodium Hydroxide, Standard Solution (0.15 N)—
7.3.1 Solution No. 1—Transfer 100 g of molybdic acid
Transfer 20 mLof the clear, supernatant stock solution to a 1-L
(85 % MoO ) to a 600–mLbeaker containing 240 mLof water
flask. Dilute to the mark with freshly boiled and cooled water
and mix thoroughly. Add 140 mL of NH OH while stirring
and mix thoroughly. Standardize this solution against potas-
vigorously. When dissolution is complete, filter through a
sium acid phthalate. It is convenient to adjust the normality of
medium paper, add 60 mL of HNO , and cool.
this standard solution to 0.148 N (1 mL = 0.0002 g P). Confirm
7.3.2 Solution No. 2—Add 400 mL of HNO to 960 mL of
the phosphorus value by analyzing a standard of a known
water in a 2-L beaker and cool.
phosphorus content, preferably an iron ore of similar compo-
7.3.3 Add Solution No. 1 to Solution No. 2 while stirring
sition. Protect the NaOH solution from CO by means of a
constantly. Add 0.1 g of ammonium phosphate, dibasic
soda-lime or soda-asbestos tube.
((NH ) HPO ), and let stand at least 24 h before using. Use
4 2 4
7.19 Sulfurous Acid (H SO ).
2 3
only the clear supernatant liquid.
7.4 Ammonium Nitrate (NH NO )
4 3
8. Hazards
7.5 Ferric Chloride Solution—Dissolve 0.3 g of pure iron
8.1 For precautions to be observed in this test method, refer
wire in 25 mL of HCl (1 + 1). Oxidize by adding HNO
to Practices E50.
dropwise to the hot solution. Cool, add 25 mLof HCl, dilute to
1 L and mix.
9. Sampling and Sample Preparation
7.6 Ferrous Sulfate Solution—Dissolve 100 g of ferrous
9.1 Sampling—The gross sample shall be collected and
sulfate (FeSO ·7H O) in 1 L of H SO (5 + 95).
4 2 2 4 prepared in accordance with Practice E877.
7.7 Hydrobromic Acid (1 + 4)—Mix 20 mL of concentrated
9.2 Sample Preparation—The laboratory sample shall be
hydrobromic acid (HBr, sp gr 1.49) with 80 mL of water.
pulverized to pass a No. 100 (150-µm) sieve.
7.8 Hydrochloric Acid (1 + 1)—Mix equal volumes of con-
NOTE 1—Some ores, such as specular hematites, may require finer
centrated HCl (sp gr 1.19) and water.
grinding to pass a No. 200 (75-µm) sieve.
7.9 Hydrofluoric Acid (sp gr 1.15)—Concentrated HF.
9.3 Sample Weight—Weigh approximately (within
6 25 mg) an amount of sample specified as follows:
7.10 Nitric Acid, Standard (0.15 N)—Transfer 10 mL of
Content of Phosphorus, % Weight of Sample, g
clear and water white concentrated HNO (sp gr 1.42) to a 1-L
flask, dilute to the mark, and mix. Standardize this solution
0.01 to 0.10 2.0
against the standard sodium hydroxide (NaOH) solution using
0.11 to 0.50 1.0
0.51 to 1.00 0.5
phenolphthalein as indicator. If desired, this solution may be
made equivalent to the standard sodium hydroxide solution by
10. Procedure
dilution with water.
10.1 Transfer the test sample to a small dry weighing bottle
7.11 Nitric Acid, Wash Solution (1 + 99)—Mix 10 mL of
andplaceinadryingoven.Afterdryingat105 °Cto110 °Cfor
concentrated HNO (sp gr 1.42) with 990 mL of water.
1 h, cap the bottle, and cool to room temperature in a
7.12 Perchloric Acid (70 %) (HClO ).
desiccator. Moment
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1 ´1
Designation: E278 − 01 (Reapproved 2010) E278 − 01 (Reapproved 2015)
Standard Test Method for
Determination of Phosphorus in Iron Ores by
Phosphomolybdate Coprecipitation and Nitric Acid
Titrimetry
This standard is issued under the fixed designation E278; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Editorial corrections were made throughout in June1.2 2010.and Table 1.
1. Scope
1.1 This test method covers the determination of phosphorus in iron ores, concentrates, and agglomerates.
1.2 This test method covers the determination of phosphorus in the concentration range from 0.01 % to 1.00 %.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
E50 Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E877 Practice for Sampling and Sample Preparation of Iron Ores and Related Materials for Determination of Chemical
Composition and Physical Properties
E882 Guide for Accountability and Quality Control in the Chemical Analysis Laboratory
3. Terminology
3.1 Definitions—For definitions of terms used in this test method, refer to Terminology E135.
4. Summary of Test Method
4.1 The sample is dissolved in HCl and HNO . After the addition of HClO , the solution is evaporated to strong fumes to
3 4
dehydrate the silica. The insoluble residue is filtered off, ignited, and treated for the recovery of any contained phosphorus.
Ammonium molybdate is added to precipitate phosphomolybdate. The precipitate is filtered off and washed free from acid. It is
then dissolved in an excess of standard sodium hydroxide solution. The excess sodium hydroxide is titrated with a standard solution
of HNO using phenolphthalein as an indicator.
5. Significance and Use
5.1 This test method is intended to be used for compliance with compositional specifications for phosphorus content. It is
assumed that all who use these procedures will be trained analysts capable of performing common laboratory procedures skillfully
and safely. It is expected that work will be performed in a properly equipped laboratory and that proper waste disposal procedures
will be followed. Appropriate quality control practices shall be followed, such as those described in Guide E882.
This test method is under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and is the direct responsibility of
Subcommittee E01.02 on Ores, Concentrates, and Related Metallurgical Materials.
Current edition approved June 15, 2010Nov. 15, 2015. Published August 2010 December 2015. Originally approved in 1965. Last previous edition approved in 20052010
ɛ1
as E278 – 01 (2005).(2010) . DOI: 10.1520/E0278-01R10.10.1520/E0278-01R15E01.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
E278 − 01 (Reapproved 2015)
6. Interferences
6.1 Vanadium and arsenic, elements commonly found in iron ores, coprecipitate with the phosphorus. Provisions for their
removal or elimination of their interference are included in this test method.
6.2 Titanium tends to form an insoluble compound with phosphorus and thus may cause low values for phosphorus. Provision
for its removal is included in this test method.
7. Reagents and Materials
7.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where such
specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficient high purity
to permit its use without lessening the accuracy of the determination.
7.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water as defined by
Type II of Specification D1193.
7.3 Ammonium Molybdate Solution (Acidic).
7.3.1 Solution No. 1—Transfer 100 g of molybdic acid (85 % MoO ) to a 600–mL beaker containing 240 mL of water and mix
thoroughly. Add 140 mL of NH OH while stirring vigorously. When dissolution is complete, filter through a medium paper, add
60 mL of HNO , and cool.
7.3.2 Solution No. 2—Add 400 mL of HNO to 960 mL of water in a 2-L beaker and cool.
7.3.3 Add Solution No. 1 to Solution No. 2 while stirring constantly. Add 0.1 g of ammonium phosphate, dibasic
((NH ) HPO ), and let stand at least 24 h before using. Use only the clear supernatant liquid.
4 2 4
7.4 Ammonium Nitrate (NH NO )
4 3
7.5 Ferric Chloride Solution—Dissolve 0.3 g of pure iron wire in 25 mL of HCl (1 + 1). Oxidize by adding HNO dropwise
to the hot solution. Cool, add 25 mL of HCl, dilute to 1 L and mix.
7.6 Ferrous Sulfate Solution—Dissolve 100 g of ferrous sulfate (FeSO ·7H O) in 1 L of H SO (5 + 95).
4 2 2 4
7.7 Hydrobromic Acid (1 + 4)—Mix 20 mL of concentrated hydrobromic acid (HBr, sp gr 1.49) with 80 mL of water.
7.8 Hydrochloric Acid (1 + 1)—Mix equal volumes of concentrated HCl (sp gr 1.19) and water.
7.9 Hydrofluoric Acid (sp gr 1.15)—Concentrated HF.
7.10 Nitric Acid, Standard (0.15 N)—Transfer 10 mL of clear and water white concentrated HNO (sp gr 1.42) to a 1-L flask,
dilute to the mark, and mix. Standardize this solution against the standard sodium hydroxide (NaOH) solution using
phenolphthalein as indicator. If desired, this solution may be made equivalent to the standard sodium hydroxide solution by dilution
with water.
7.11 Nitric Acid, Wash Solution (1 + 99)—Mix 10 mL of concentrated HNO (sp gr 1.42) with 990 mL of water.
7.12 Perchloric Acid (70 %) (HClO ).
7.13 Phenolphthalein Indicator Solution—Dissolve 0.2 g of phenolphthalein in 100 mL of ethanol.
7.14 Potassium Nitrate, Wash Solution (10 g ⁄L)—Dissolve 10 g of potassium nitrate (KNO ) in water, dilute to 1 L, and mix.
7.15 Potassium Permanganate Solution (25 g ⁄L)—Dissolve 25 g of potassium permanganate (KMnO ) in water and dilute to
1 L.
7.16 Sodium Carbonate (Na CO ).
2 3
7.17 Sodium Hydroxide, Stock Solution—Dissolve 300 g of NaOH in 1 L of water. Add a slight excess of barium hydroxide
(Ba(OH) ) to precipitate any carbon dioxide (CO ). Allow any precipitate to settle out. Store the solution in a polyethylene
2 2
container.
7.18 Sodium Hydroxide, Standard Solution (0.15 N)—Transfer 20 mL of the clear, supernatant stock solution to a 1-L flask.
Dilute to the mark with freshly boiled and cooled water and mix thoroughly. Standardize this solution against potassium acid
phthalate. It is convenient to adjust the normality of this standard solution to 0.148 N (1 mL = 0.0002 g P). Confirm the phosphorus
value by analyzing a standard of a known phosphorus content, preferably an iron ore of similar composition. Protect the NaOH
solution from CO by means of a soda-lime or soda-asbestos tube.
7.19 Sulfurous Acid (H SO ).
2 3
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC, www.chemistry.org. For suggestions on the testing of
reagents not listed by the American Chemical Society, see the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD, http://www.usp.org.
´1
E278 − 01 (Reapproved 2015)
8. Hazards
8.1 For precautions to be observed in this test method, refer to Practices E50.
9. Sampling and Sample Preparation
9.
...