GB/T 1510-2016 English PDF (GBT1510-2016)

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GB/T 1510-2016: Manganese ores -- Determination of aluminium content -- EDTA titrimetric method
GB/T 1510-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 73.060.20
D 32
Replacing GB/T 1510-2006
Manganese ores - Determination of aluminium content
- EDTA titrimetric method
ISSUED ON: AUGUST 29, 2016
IMPLEMENTED ON: JULY 01, 2017
Issued by: General Administration of Quality Supervision, Inspection
and Quarantine;
Standardization Administration of the People’s Republic of
China.
Table of Contents
Foreword ... 3 
1 Scope ... 5 
2 Normative references ... 5 
3 Principle ... 5 
4 Reagents and materials ... 6 
5 Instruments ... 8 
6 Sampling ... 8 
7 Analysis steps ... 8 
8 Calculation of analysis results ... 10 
9 Test report ... 13 
Appendix A (Normative) Sample analysis value acceptance procedure flow
chart ... 14 
Manganese ores - Determination of aluminium content
- EDTA titrimetric method
WARNING – The personnel who uses this Standard shall have hands-on
experience in formal laboratory work. This Standard does not address all
possible security issues. It is the responsibility of the user to take
appropriate safety and health measures and to ensure compliance with
the conditions which are set by the relevant national regulations.
1 Scope
This Standard specifies the determination of aluminium content in manganese
ores by EDTA titrimetric method.
This Standard applies to the determination of aluminium content in manganese
ores and manganese concentrates; the determination range (mass fraction):
0.10% ~ 12.50%.
2 Normative references
The following referenced documents are indispensable for the application of
this document. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any
amendments) applies.
GB/T 2011, Method of sampling and sample preparation of manganese ores
in bulk
GB/T 6682, Water for analytical laboratory use - Specification and test
methods
GB/T 8170, Rules of rounding off for numerical values and expression and
judgment of limiting values
GB/T 14949.8, Manganese ores - Determination of hygroscopic moisture
content - Gravimetric method
3 Principle
For the sample, use hydrochloric acid-nitric acid to decompose, and use sulfuric
acid-hydrofluoric acid to evaporates silicon. After precipitation and separation
by hexamethylenetetramine, use hydrochloric acid to dissolve the aluminium
hydroxide precipitate; use sodium carbonate-boric acid to melt the residue.
After separation by strong base, divide the filtrate into the slightly acidic solution;
then, add excess EDTA. When the pH value is 5 ~ 5.5, use xylenol orange as
indicator; use zinc standard titration solution to titrate excess EDTA; use fluoride
ion to replace the EDTA with aluminium; then, use zinc standard titration
solution to titrate. According to the consumption of zinc standard titration
solution, calculate the aluminium content.
4 Reagents and materials
In the analysis process, only use approved analytical reagents and water of
grade 3 and above in accordance with GB/T 6682.
4.1 Mixed solvent: the mass ratio of sodium carbonate and boric acid is 2:1;
grind and mix well.
4.2 Nitric acid, ρ = 1.42 g/mL.
4.3 Hydrochloric acid, ρ = 1.19 g/mL.
4.4 Hydrochloric acid, 1+1.
4.5 Hydrochloric acid, 1+2.
4.6 Hydrochloric acid, 1+5.
4.7 Hydrochloric acid, 2+98.
4.8 Sulfuric acid: 1+1.
4.9 Hydrofluoric acid, ρ = 1.17 g/mL.
4.10 Hydrogen peroxide, mass fraction of 30%.
4.11 Ammonia water, 1+1.
4.12 Hydrochloric acid-hexamethylenetetramine solution (pH = 5 ~ 5.5): Weigh
40 g of hexamethylenetetramine and dissolve it in water; add 20 mL of
hydrochloric acid (1+1); use water to dilute to 100 mL; mix well.
4.13 Hexamethylenetetramine solution, 5 g/L.
4.14 Sodium hydroxide solution, 500 g/L: Weigh 500 g of sodium hydroxide;
use water to dissolve and dilute to 1 L; store in a plastic bottle.
4.15 Sodium fluoride saturated solution: Store in a plastic bottle.
7.4 Determination
7.4.1 Preparation of sample solutions
7.4.1.1 Put the sample (see 7.2) in a 400 mL beaker; add 20 mL of hydrochloric
acid (see 4.3); heat the solution until there is no obvious reaction,; then, add 5
mL of nitric acid (see 4.2). Continue to heat to dissolve until nearly dry; remove
and cool slightly; add 20 mL of hydrochloric acid (see 4.4) and 100 mL of water;
heat to dissolve the salts. Remove it; use medium-speed filter paper to filter
while it is still hot; use hot water to wash the filter paper 10 ~ 15 times. Keep
the filtrate as main liquid A.
7.4.1.2 Transfer the filter paper and residue into a platinum dish or platinum
crucible; dry and carbonize at low temperature; put it into a high temperature
furnace at about 550 °C for ashing; then, burn it in a high temperature furnace
at 850 °C for 10 minutes; remove it for cooling. Add 2 mL of sulfuric acid (see
4.8); add 3 mL ~ 5 mL of hydrofluoric acid (see 4.9) dropwise; after heating to
evaporate the silicon, heat it on an electric hot plate until the sulfuric acid emits
smoke; remove it. Slightly cool; blow a small amount of water around the
platinum dish; then, heat until the sulfuric acid smokes and is almost dry.
Remove it; add 10 mL of hydrochloric acid (see 4.4); heat to dissolve the salts;
combine the test solution with the main solution A.
7.4.2 Separation of hexamethylenetetramine
7.4.2.1 Adjust the volume of the solution (see 7.4.1.2) to about 100 mL ~ 150
mL; boil and remove. Use ammonia water (see 4.11) to neutralize until a
precipitation occurs; then, use hydrochloric acid (see 4.4) to adjust until the
precipitate just dissolves; add 5 ~ 10 drops in excess. Add 20 mL of hydrochloric
acid-hexamethylenetetramine solution (see 4.12); heat to slightly boil and keep
at a temperature (80 °C ~ 90 °C) for 15 min ~ 20 min. Remove and cool slightly;
use a medium-speed filter paper to filter (in two funnels when there are a lot of
precipitations of hydroxide of iron and aluminium); use hot
hexamethylenetetramine solution (see 4.13) to wash the beaker and precipitate
5 ~ 8 times respectively. Use 30 mL of hot hydrochloric acid (see 4.5) to dissolve
the precipitate in the original beaker; use hot hydrochloric acid (see 4.7) to wash
the filter paper until it is no longer yellow; then, use hot water to wash the filter
paper for 10 ~ 15 times. Keep the solution as the main liquid B for strong base
separation.
7.4.2.2 Transfer the filter paper and residue into a platinum dish or platinum
crucible; put it into a high temperature furnace at about 550 °C for ashing; then,
burn it in a high temperature furnace at 850 °C for 10 minutes; remove it for
cooling. Add 3 g of mixed solvent (see 4.1); put it in a high temperature furnace
of 950 °C for 10 min; take it out and cool it slightly; add hydrochloric acid (see
4.4) dropwise; heat until the frit is separated from the platinum crucible; pour it
into the main liquid B and combine them.
7.4.3 Strong base separation
Heat and evaporate the solution (see 7.4.2.2) to a volume of about 80 mL ~ 120
mL; add 10 mL of sodium hydroxide solution (see 4.14); use ammonia water
(see 4.11) to neutralize until a precipitation occurs; then, use hydrochloric acid
(see 4.4) to adjust until the precipitate dissolves, and exceed for 10 mL; boil for
1 min ~ 2 min. Remove it and cool it down; add 40 mL of sodium hydroxide
solution (see 4.14) at one time under constant stirring; add 8 ~ 10 drops of