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GB/T 1509-2016 PDF in English

GB/T 1509-2016 (GB/T1509-2016, GBT 1509-2016, GBT1509-2016)
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GB/T 1509-2016: PDF in English (GBT 1509-2016)

GB/T 1509-2016
ICS 73.060.20
D 32
Replacing GB/T 1509-2006
Manganese ores - Determination of silicon content -
Perchloric acid dehydration gravimetric method
(ISO 5890:1981, Manganese ores and concentrates - Determination of silicon
content - Gravimetric method, MOD)
Issued by: General Administration of Quality Supervision Inspection and
Quarantine of PRC;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3 
1 Scope ... 6 
2 Normative references ... 6 
3 Principles ... 6 
4 Reagents and materials ... 7 
5 Instruments ... 7 
6 Sampling and preparation ... 7 
7 Analytical procedures ... 7 
8 Calculation of results ... 10 
9 Test report ... 11 
Appendix A (Normative) The flowchart of acceptance procedure of sample’s
analytical value ... 13 
Manganese ores - Determination of silicon content -
Perchloric acid dehydration gravimetric method
Warning - The personnel using this standard shall have practical
experience in formal laboratory work. This standard does not point out all
possible safety issues. The user is responsible for taking appropriate
safety and health measures and ensuring compliance with the conditions
stipulated by relevant national laws and regulations.
1 Scope
This standard specifies the determination of silicon content in manganese ore
by the perchloric acid dehydration gravimetric method.
This standard applies to the determination of silicon content in fluorine-free
manganese ores and manganese concentrates; the measurement range (mass
fraction): 0.50% to 20.00%.
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) are applicable to this standard.
GB/T 2011 Method of sampling and sample preparation of manganese ores
in bulk (GB/T 2011-1987, neqISO3081:1983)
GB/T 6682 Water for analytical laboratory use - Specification and test
methods (GB/T 6682-2008, ISO 3696:1987, MOD)
GB/T 8170 Rules of rounding off for numerical values & expression and
judgement of limiting values
GB/T 14949.8 Manganese ores - Determination of hygroscopic moisture
content in analytical samples (GB/T 14949.8-1994, eqv ISO 310:1981)
3 Principles
The sample is decomposed by hydrochloric acid and nitric acid, filtered; the
residue is melted by sodium carbonate; the leaching liquid is combined with the
main liquid; perchloric acid is added to dehydrate the silicic acid; the precipitate
is burnt, weighed, volatilized by hydrofluoric acid to remove the silicon. It is burnt
and weighed. The mass difference before and after the treatment by
hydrofluoric acid is used to calculate the silicon content.
4 Reagents and materials
In the analysis process, only use approved analytical reagents and water that
meets the grade 3 or higher purity as specified in GB/T 6682.
4.1 Anhydrous sodium carbonate, solid.
4.2 Hydrochloric acid, ρ = 1.19 g/mL.
4.3 Hydrochloric acid, 1 + 4.
4.4 Hydrochloric acid, 1 + 9.
4.5 Nitric acid, ρ = 1.40 g/mL.
4.6 Sulfuric acid, 1 + 1.
4.7 Perchloric acid, ρ = 1.67 g/mL.
4.8 Hydrofluoric acid, ρ = 1.15 g/mL.
4.9 Hydrogen peroxide, ρ = 1.11 g/mL.
4.10 Ammonium thiocyanate solution, 50 g/L.
5 Instruments
Common laboratory instruments and equipment are used in the analysis.
6 Sampling and preparation
According to GB/T 2011, take sample and prepare it. The particle size of the
sample shall not be greater than 0.080 mm.
7 Analytical procedures
7.1 Number of analyses
Perform at least two repeatability analyses on the same sample.
7.4.3 Separation of silicon
Add 30 mL of perchloric acid (see 4.7) to the solution obtained in 7.4.2. Heat
and evaporate until the white smoke of perchloric acid begins to be emitted.
Cover with a watch glass. Continue to heat until the perchloric acid is refluxed
for 15 to 20 minutes. Remove it. Cool the solution. Add 40 mL ~ 50 mL of hot
water, 2 ~ 3 drops of hydrogen peroxide (see 4.9). Add 5 mL of hydrochloric
acid (see 4.2). Heat to dissolve soluble salts until the solution is clear.
Immediately use medium-speed quantitative filter paper with a little pulp to filter
it. Use a glass rod with a rubber tip to transfer the silicon precipitate in the
beaker to the filter paper.
First use cold water to wash the beaker and the precipitate 2 ~ 3 times. Then
use hot hydrochloric acid (see 4.4) to wash it, until there is no iron ions (test
with ammonium thiocyanate solution (see 4.10), if the ammonium thiocyanate
solution turns red, it indicates that there is still iron ion]. Finally use cold water
to wash it 2 ~ 3 times. For samples with silicon content (mass fraction) below
10%, discard the filtrate and washing liquid. For samples with a silicon content
(mass fraction) of more than 10%, add 20 mL of perchloric acid (see 4.7) to the
filtrate. Repeat evaporation and smoking, filtration, washing; the resulting
precipitate is processed according to operation step 7.4.4.
Note 1: The surface of the solution is calm when heating and evaporating to the
beginning of white smoke of perchloric acid.
Note 2: There is a downward flow on the cup wall during the reflux of the perchloric
acid smoke; the solution gradually forms a gel.
7.4.4 Treatment of silicon precipitate
Put the precipitate together with the filter paper in a platinum crucible. At low
temperature, heat to dry and carbonize it. Place it in a high temperature furnace
at 700 °C ~ 750 °C for ashing. Then increase the temperature to 950 °C ~
1000 °C. Burn to a constant amount. Take it out. Place it in a desiccator. Cool
to room temperature. Weigh the mass of the crucible and the precipitate (m1).
Use a few drops of water to wet the precipitate in the platinum crucible. Add 5
~ 10 drops of sulfuric acid (see 4.6), 5 mL to 10 mL of hydrofluoric acid (see
4.8). Slowly evaporate on an electric furnace until silicon and sulfuric acid are
completely volatilized. Place the platinum crucible containing the residue in a
high temperature furnace at 950 °C ~ 1000 °C and burn to a constant amount.
Take it out. Place it in a desiccator. Cool to room temperature. Weigh the
crucible and the mass of the residue (m2).
Note: When silicon and sulfuric acid are completely volatilized, there will be no
more smoke in the platinum crucible.
8.2.2 Acceptance of analytical values of standard samples
When analyzing the sample, it is necessary to analyze the same type of
standard sample along with the sample. The analytical value of the standard
sample shall meet the conditions of formula (2):
y - The analytical value of the standard sample;
µ0 - The definite standard value of the standard sample;
k3 - 0.7, the critical difference coefficient;
R - Allowable difference.
If the analytical value of the standard sample does not conform to formula (2),
it needs to be re-analyzed together with the sample.
If the two analytical values of the sample exceed the allowable error limit given
in Table 2, one or more additional analyses shall be performed simultaneously
with the standard sample of the same type of ore according to the flowchart in
Appendix A.
In any case, the acceptability of the analytical value of the sample shall depend
on the acceptability of the analytical value of the standard sample.
8.2.3 Calculation of final result
The final result is the arithmetic average of the acceptable value of the sample,
or the analytical value of the sample obtained according to the process specified
in Appendix A. The value is rounded off according to the provisions of GB/T
8170, retaining two decimal places.
9 Test report
The test report shall include the following:
a) The name and address of the testing laboratory;
b) Date of release of test report;
c) The number of this standard;
d) The necessary detailed description of the sample itself;
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.