GB/T 4701.1-2009Ferrotitanium - Determination of titanium content - The ammonium ferric sulfate titration method (English PDF)
钛铁 钛含量的测定 硫酸铁铵滴定法
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Issued by
SAMR; SAC
Level / Type
National · Recommended
Issue date
October 30, 2009
Implementation date
May 1, 2010
Scope
GB/T 4701.1-2009 is the English-translated version of 钛铁 钛含量的测定 硫酸铁铵滴定法.
GB/T 4701.1-2009 specifies the determination of the titanium content of ferrotitanium by the ammonium ferric sulfate titration method.
Clause 1 states that this part of GB/T 4701 applies to the determination of titanium in ferrotitanium over a measuring range of 20.00% to 80.00% mass fraction, and a caution placed before it warns that users must have practical experience in laboratory work and that the part does not address all safety problems, the user remaining responsible for taking safety and health measures and for compliance with the relevant national regulations.
Clause 2 cites GB/T 4010 on the sampling and preparation of ferroalloy samples for chemical analysis.
Clause 3 sets out the principle: the sample is dissolved with sulfuric, nitric, hydrochloric and hydrofluoric acids; where chromium, vanadium, molybdenum or tin interfere, titanium hydroxide is precipitated in the presence of hydrogen peroxide to separate the titanium from them; the titanium is then reduced to the trivalent state with metallic aluminium under carbon dioxide or nitrogen, titrated with a standard titration solution of ammonium ferric sulfate against a thiocyanate indicator, and calculated from the volume consumed.
Clause 4 lists the reagents and materials, among them titanium-free aluminium foil 0.10 mm thick with Al not less than 99.5%, oxygen-free nitrogen and carbon dioxide of 99.99% purity, ammonium thiocyanate solution at 100 g/L, an ammonium ferric sulfate solution at 35 g/L containing about 4 mg of iron per millilitre, and a titanium standard solution prepared from titanium dioxide of at least 99.9% titanium previously burned at 800 degrees C for 2 h.
The rest of the document, as the table of contents gives it, is made up of Instruments, Sampling and preparation of samples, Analytical procedures, Calculation of analytical result, Allowable difference and Test report.
The draft on the page skips from the reagent list to the analytical procedure in 7.3, which takes a 50.00 mL aliquot of the test solution when the titanium content is expected to be 20% to 45% and a 25.00 mL aliquot when it is 45% to 75%, in one version for samples free of interfering elements and one that separates them by precipitation and filtration, and then reduces the titanium with sodium bicarbonate and aluminium foil under cover; the page breaks off in that subclause.
It replaces GB/T 4701.1-1984, was issued on October 30, 2009 and has applied since May 1, 2010.
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Document preview — GB/T 4701.1-2009
National Standard of the People's Republic of China
- ICS
- 77.100
- Classification
- H 11
- Replacing
- GB/T 4701.1-1984
Issued by: State Administration for Market Regulation; Standardization Administration of the PRC
Contents
- Foreword3
- 1 Scope4
- 2 Normative references4
- 3 Principles4
- 4 Reagents and materials5
- 5 Instruments7
- 6 Sampling and preparation of samples8
- 7 Analytical procedures8
- 8 Calculation of analytical result10
- 9 Allowable difference11
- 10 Test report11
1 Scope
This Part of GB/T 4701 specifies the determination of titanium content in ferrotitanium using the ammonium ferric sulfate titration method.
This Part applies to the determination of titanium content in ferrotitanium. Measuring range (mass fraction). 20.00%~80.00%.
2 Normative references
The clauses in the following documents, by reference in this Part of GB/T 4701, constitute the clauses of this Part. For the dated references, the subsequent amendments (not including errata content) or revisions do not apply to this Part. However, parties which have reached an agreement according to this Part are encouraged to study whether the latest version of these documents can be used. For the undated references, the latest version is applicable to this Part.
GB/T 4010 Ferroalloys sampling and preparation of samples for chemical analysis
3 Principles
The sample is dissolved with sulfuric acid, nitric acid, hydrochloric acid, and hydrofluoric acid. If there are chromium, vanadium, molybdenum, and tin interfering elements, in the presence of hydrogen peroxide, the titanium hydroxide can be precipitated to separate from the interfering elements. In a carbon dioxide or nitrogen atmosphere, the titanium is reduced to trivalence with metallic aluminum. USE thiocyanate as an indicator; TITRATE with a standard titration solution of ammonium ferric sulfate; according to the consumption of the standard titration solution of ammonium ferric sulfate, CALCULATE the content of titanium in the sample.
4 Reagents and materials
Unless otherwise stated, in the analysis, only reagents and distilled water identified as analytical purity or water equivalent to the purity shall be used.
4.1 Aluminum, (Al>=99.5%), thickness of 0.10 mm, aluminum foil without titanium. When used, 1 g of aluminum foil is folded to form a rectangle of about 3 cm~4 cm in length and about 1 cm in width.
4.2 Sodium bicarbonate, solid.
4.3 Sulfuric acid, rho1.84 g/mL.
4.4 Nitric acid, rho1.42 g/mL.
4.5 Hydrochloric acid, rho1.19 g/mL.
4.6 Hydrofluoric acid, rho1.15 g/mL.
4.7 Hydrogen peroxide, rho1.10 g/mL.
4.8 Sulfuric acid, 1+1.
4.9 Sulfuric acid, 1+4.
4.10 Sodium hydroxide solution, 100 g/L, stored in plastic bottle.
4.11 Sodium hydroxide solution, 20 g/L, stored in plastic bottle.
4.12 Ammonium thiocyanate solution, 100 g/L.
4.13 Nitrogen, oxygen free (oxygen content less than 10 x 10^-6 by volume), purity 99.99%.
4.14 Carbon dioxide, oxygen free (oxygen content less than 10 x 10^-6 by volume), purity 99.99%.
4.15 Ammonium ferric sulfate solution, 35 g/L. WEIGH 35 g of ammonium ferric sulfate [NH4Fe(SO4)2 . 12H2O]; PLACE it in a 400 mL beaker; ADD 100 mL of water and 100 mL of sulfuric acid (1+1); after dissolving, TRANSFER to a 1000 mL volumetric flask; and USE water to dilute to volume, MIX well. This solution contains about 4 mg of iron in 1 mL.
4.16 Titanium standard solution
WEIGH 0.8340 g of titanium dioxide (Ti>=99.9%) which was previously burned at 800 °C for 2 h; PLACE in a platinum crucible with a platinum cover; ADD 10 with a Teflon watch glass; and slowly ADD 5 mL of nitric acid (4.4) to oxidize while cooling. After the reaction is completed, REMOVE the watch glass; HEAT it until sulfuric acid fumes, and CONTINUE to heat for about 5 min; REMOVE and COOL. ADD 30 mL of hydrochloric acid (4.5), and carefully STIR; COVER with the Teflon watch glass; HEAT until the solution is clear. REMOVE, and WASH the watch glass with 5 mL of hydrochloric acid (4.5); after cooling, TRANSFER to a 500 mL volumetric flask; USE water to dilute to volume, and MIX well.
7 Analytical procedures
7.3.2 Interfering elements-free
If the content of titanium in the sample is expected to be 20%~45%, PIPETTE 50.00 mL of the test solution (7.3.1). If the content of titanium is 45%~75%, PIPETTE 25.00 mL of the test solution (7.3.1). PLACE the test solution in a 500 mL conical flask; ADD 85 mL of hydrochloric acid (4.5) and 25 mL of water; and PERFORM as specified in 7.3.4 and 7.3.5 or in 7.3.4 and 7.3.6.
7.3.3 Separation of interfering elements
If the content of titanium in the sample is expected to be 20% ~ 45%, PIPETTE 50.00 mL of the test solution (7.3.1). If the content of titanium is 45%~75%, PIPETTE 25.00 mL of the test solution (7.3.1). PLACE the test solution in a 250 mL beaker containing 10 mL of ammonium ferric sulfate solution (4.15); ADD 50 mL of sodium hydroxide solution (4.10) and 2 mL of hydrogen peroxide solution (4.7); HEAT and BOIL for 5 min. After the precipitate sinks, FILTER with double-layer fast filter paper; then TRANSFER all the precipitate to the filter paper; thoroughly WASH the beaker and precipitate 6 times with about 10 mL of sodium hydroxide solution (4.11) each time; and then thoroughly WASH the filter paper and precipitate with sodium hydroxide solution (4.11). WASH the funnel neck with water; then PLACE the funnel on a 500 mL conical flask. ADD 45 mL of hydrochloric acid (4.5) and 15 mL of sulfuric acid (4.9) to the initial 250 mL beaker; and HEAT to 60 °C ~ 70 °C. The mixed acid is added to the filter paper 6 times to dissolve the precipitate (WAIT for the acid to flow away and then ADD another time). WASH the filter paper three times with 35 mL of hydrochloric acid (4.5) at 60 °C ~ 70 °C; and finally WASH the beaker, filter paper, and funnel neck with no more than 40 mL of water at 70 °C ~ 80 °C. PERFORM as specified in 7.3.4 and 7.3.5 or in 7.3.4 and 7.3.6.
7.3.4 Reduction of titanium
ADD 2 g of sodium bicarbonate (4.2) and 4 g of aluminum foil (4.1) to the test solution (7.3.2 or 7.3.3); immediately COVER it with the Bunsen valve or Gai funnel with saturated sodium bicarbonate solution. During the reduction, the solution shall be shaken constantly. […]
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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.
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Editions of GB/T 4701.1
| Edition | Title | Revision | Status |
|---|---|---|---|
| GB/T 4701.1-2009 | Ferrotitanium - Determination of titanium content - The ammonium ferric sulfate titration method | current edition | Current |
| GB/T 4701.1-1984 | Ferrotitanium - Determination of titanium content - The ammonium ferric sulfate titration method | previous edition | Superseded |
This page sells the current edition, GB/T 4701.1-2009. Earlier editions are listed for reference only.
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Related Standards
GB/T 4010-1994 — Ferroalloys-sampling and preparation of samples for chemical analysis
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GB/T 4701.2-2009 — Ferrotitanium - Determination of silicon content - The sulphuric acid dehydration gravimetric method
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