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GB/T 4698.2-2011 English PDF (GBT4698.2-2011)

GB/T 4698.2-2011 English PDF (GBT4698.2-2011)

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GB/T 4698.2-2011: Methods for chemical analysis of titanium sponge, titanium and titanium alloys -- Determination of iron content
GB/T 4698.2-2011
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.50
H 64
Replacing GB/T 4698.2-1996
Methods for chemical analysis of titanium sponge, titanium
and titanium alloys - Measurement of iron content
ISSUED ON: MAY 12, 2011
IMPLEMENTED ON: FEBRUARY 01, 2012
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of PRC;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3 
1 Scope ... 5 
2 Normative references ... 5 
3 General ... 5 
4 Method 1 -- 1,10-phenanthroline spectrophotometry ... 6 
5 Method 2 -- Atomic absorption spectrometry ... 9 
6 Method 3 -- Inductively coupled plasma atomic emission spectrometry ... 14 
Appendix A (Informative) The structural changes of this Part, as compared with ISO
22960:2008, ISO 22961:2008, ISO 22962:2008 ... 22 
Appendix B (Informative) Technical differences between method 1 of this Part and ISO
22960:2008, method 2 and ISO 22961:2008, method 3 and ISO 22962:2008 and their
reasons ... 24 
Methods for chemical analysis of titanium sponge, titanium
and titanium alloys - Measurement of iron content
1 Scope
This Part specifies the method for the measurement of iron content in sponge titanium,
titanium, titanium alloys.
This Part applies to the measurement of iron content, in sponge titanium, titanium,
titanium alloys.
2 Normative references
The following documents are essential to the application of this document. For the dated
documents, only the versions with the dates indicated are applicable to this document;
for the undated documents, only the latest version (including all the amendments) is
applicable to this standard.
GB/T 6682 Water for analytical laboratory use - Specification and test methods (ISO
3696, MOD)
GB/T 12806 Laboratory glassware - One-mark volumetric flasks (ISO 1042, EQV)
GB/T 12808 Laboratory glassware - One mark pipette (ISO 648, EQV)
GB/T 12809 Laboratory glassware - Principles of design and construction of
volumetric glassware (ISO 384, EQV)
GB/T 12810 Laboratory glassware - Volumetric glassware - Methods for use and
testing of capacity (ISO 4787, IDT)
3 General
3.1 Unless otherwise stated, only confirmed analytical pure reagents are used in the
analysis; the water used is distilled water or deionized water or water of equivalent
purity, which shall comply with the provisions of GB/T 6682.
3.2 The instruments used shall be within the calibration period. Their performance shall
meet the technical parameters, which are required by the calibration. The glass
containers shall be grade A, which is specified in GB/T 12808, GB/T 12809, GB/T
12806; the specific use method shall refer to the requirements of GB/T 12810.
4 Method 1 -- 1,10-phenanthroline spectrophotometry
4.1 Measurement range
The measurement range of iron is 0.005% ~ 2.00% (mass fraction).
4.2 Method principle
The sample is dissolved by hydrochloric acid-hydrofluoric acid. The titanium oxide
nitric acid is added. The boric acid, tartaric acid, ammonium acetate, hydroxylamine
hydrochloride is added. The 1,10-phenanthroline is added, to form 1,10-phenanthroline
iron complex; the iron content is measured by spectrophotometer.
4.3 Reagents
4.3.1 Hydrochloric acid (1 + 1): Slowly add 500 mL of hydrochloric acid (ρ1.16 g/mL
~ 1.19 g/mL), into 500 mL water.
4.3.2 Nitric acid (1 + 1): Slowly add 500 mL of nitric acid (ρ1.42 g/mL), into 500 mL
of water.
4.3.3 Hydrofluoric acid (1 + 1): Carefully and slowly add 100 mL of hydrofluoric acid
(ρ1.14 g/mL), into 100 mL of water.
4.3.4 Boric acid.
4.3.5 Tartaric acid (200 g/L).
4.3.6 Ammonium acetate (500 g/L).
4.3.7 Hydroxylamine hydrochloride solution (100 g/L).
4.3.8 The 1,10-phenanthroline solution (2 g/L): Dissolve 2.0 g of 1,10-phenanthroline
in 100 mL of ethanol (volume percentage not less than 95%). Use water to dilute it to
1000 mL.
4.3.9 Iron standard solution
4.3.9.1 Iron standard storage solution (0.500 mg/mL): Accurately weigh 0.500 g of
metallic iron (wFe ≥ 99.9%), into a 300 mL beaker (accurate to 0.0001 g). Add 30 mL
of hydrochloric acid (4.3.1). Heat to dissolve it. Add 5 mL of nitric acid (4.3.2), to
oxidize iron. Continue to heat, to drive off nitrogen oxides. Cool it down. Transfer to a
1000 mL volumetric flask. Use water to dilute it to the mark. Mix well.
4.3.9.2 Iron standard solution (0.050 mg/mL): Pipette 10.00 mL of iron standard stock
solution (4.3.9.1), into a 100 mL volumetric flask. Use water to dilute it to the mark.
5.3.4 Boric acid.
5.3.5 Pure titanium
wTi ≥ 99.95%; the iron content is known AND shall be as low as possible. If the iron
content is unknown, it shall use the method 1 for accurate measurement.
5.3.6 Iron standard solution
5.3.6.1 Iron standard stock solution (0.500 mg/mL)
Weigh 0.500 g of metallic iron [wFe ≥ 99.9%], into a 300 mL beaker (accurate to 0.0001
g). Add 30 mL of hydrochloric acid (5.3.1). Heat to dissolve it. Add 5 mL of nitric acid
(5.3.2), to oxidize the iron. Continue to heat to drive off nitrogen oxides. Cool it down.
Transfer it into a 1000 mL volumetric flask. Use water to dilute it to the mark. Mix well.
5.3.6.2 Iron standard solution (0.050 mg/mL)
Pipette 10.00 mL of iron standard stock solution (5.3.6.1) into a 100 mL volumetric
flask. Use water to dilute it to the mark. Mix well. Prepare it when using.
5.4 Instruments
5.4.1 Analytical balance: Accurate to 0.1 mg.
5.4.2 Flame atomic absorption spectrometer: It uses air/acetylene flame; the wavelength
is 248.3 nm.
5.5 Specimen
5.5.1 Specimen requirements
Sampling of sponge titanium, titanium, titanium alloys shall be carried out, in
accordance with published standard methods.
5.5.2 Sample
Weigh 0.50 g of sample, accurate to 0.0001 g.
5.6 Analytical procedures
WARNING: Air-acetylene burners shall be ignited and extinguished, in
accordance with atomic absorption spectrometry instrumentation procedures, to
avoid a possible explosion hazard.
5.6.1 Number of measurements
Two samples are measured independently. Take the average value.
5.6.2 Blank test
Carry out the blank test, by the use of pure titanium (5.3.5), along with the sample.
5.6.3 Preparation of standard solutions
5.6.3.1 General
The preparation of standard solution is carried out, according to 5.6.3.2 and 5.6.3.3.
5.6.3.2 wFe ≤ 0.1%
5.6.3.2.1 Weigh 6 parts of pure titanium (5.3.5), 0.50 g per each part. Place them in a
200 mL polyethylene beaker.
5.6.3.2.2 Add 10 mL of hydrochloric acid (5.3.1) and 5 mL of hydrofluoric acid (5.3.3).
Cover a polyethylene watch glass. Heat in a water bath to dissolve it. Add 3 mL of nitric
acid (5.3.2). Heat to drive off nitrogen oxides. Add 3 g of boric acid (5.3.4). Stir to
dissolve it. Cool it to room temperature.
5.6.3.2.3 Transfer the solution into a 100 mL volumetric flask. Add 0.00 mL, 2.00 mL,
4.00 mL, 6.00 mL, 8.00 mL, 10.00 mL of iron standard solution (5.3.6.2), respectively.
Use water to dilute it to the mark. Mix well.
5.6.3.3 wFe > 0.1%
5.6.3.3.1 Weigh 6 parts of pure titanium (5.3.5), 0.50 g per each part. Place them in a
200 mL polyethylene beaker.
5.6.3.3.2 Add 10 mL of hydrochloric acid (5.3.1) and 5 mL of hydrofluoric acid (5.3.3).
Cover a polyethylene watch glass. Heat in a water bath to dissolve it. Add 3 mL of nitric
acid (5.3.2). Continue to heat to drive off nitrogen oxides. Add 3 g of boric acid (5.3.4).
Stir to dissolve it. Cool it to ...
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