GB/T 1506-2016 PDF English
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Manganese ores - Determination of manganese content - Potentiometric method and ammonium iron (II) sulphate titrimetric method
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| GB/T 1506-2002 | English | 359 |
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Manganese ores -- Determination of manganese content -- Potentiometric method and ammonium iron (Ⅰ) sulphate titrimetric method
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| GB/T 1506-1979 | English | 199 |
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Method for determination of total manganese content in manganese ores
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GB/T 1506-2016: Manganese ores - Determination of manganese content - Potentiometric method and ammonium iron (II) sulphate titrimetric method
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GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 73.060.20
D 32
Replacing GB/T 1506-2002
Manganese ores - Determination of manganese
content - Potentiometric method and ammonium
iron (II) sulphate 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 PRC.
Table of Contents
Foreword... 3
1 Scope... 5
2 Normative references... 5
3 Method 1.Potentiometric titration... 6
4 Method 2.ammonium iron (II) sulphate titrimetric method... 11
5 General processing of analysis results... 16
6 Test report... 17
Appendix A (Normative) Specimen analysis value acceptance procedure flow
chart... 18
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard replaces GB/T 1506-2002 “Manganese ores - Determination of
manganese content - Potentiometric method and ammonium iron (II) sulphate
titrimetric method”.
As compared with GB/T 1506-2002, the main technical changes are as follows.
- ADD the content of normative references;
- MODIFY the expression of requirements for the reagents and water used;
- ADD the contents of the reagents used;
- ADD the provisions on the number of determinations;
- MODIFY the operational statement of the blank value determination;
- MODIFY the added water volume for the preparation of N-phenyl anthranilic
acid indicator solution (0.2 g/L);
- MODIFY the operational statement of the dissolution of the sample by
ammonium nitrate oxidation;
- MODIFY the operational statement of the dissolution of the sample by
perchloric acid oxidation;
- MODIFY the amount of nitric acid added when the sample is dissolved by
perchloric acid oxidation;
- ADD notes on the applicability of the two sample dissolution methods;
- MODIFY the operational statement before titration with ammonium ferrous
sulfate standard solution;
- ADD the acceptance of the analytical value of the standard sample;
- ADD the calculation of the final result;
- ADD the requirements for the test report;
- ADD Appendix A.
This standard was proposed by the China Iron and Steel Association.
This standard shall be under the jurisdiction of the National Standards
Committee for Pig Iron and Ferroalloys (SAC/TC 318).
Drafting organizations of this standard. Angang Mining Group, Changsha
Mining and Metallurgy Research Institute Co., Ltd., Metallurgical Industry
Information Standards Institute.
The main drafters of this standard. Tian Hong, Chen Zhihua, Gao Jingjun,
Zhang Bin, Yang Lin, Sun Deming, Wang Dan, Ma Caiyun, Lu Chunsheng.
This standard replaces the standard previously issued as follows.
- GB/T 1506-1979, GB/T 1506-2002.
Manganese ores - Determination of manganese
content - Potentiometric method and ammonium
iron (II) sulphate titrimetric method
Warning - The personnel using this standard shall have practical
experience in formal laboratory work. This standard does not address all
possible safety issues. It is the responsibility of the user to take
appropriate safety and health measures and to ensure compliance with
the conditions set by the relevant national regulations.
1 Scope
This standard specifies the determination of manganese in manganese ore by
potentiometric method and ammonium iron (II) sulphate titrimetric method.
This standard is applicable to the determination of manganese content in
manganese ore and manganese concentrates with vanadium content (mass
fraction) not more than 0.05%, the determination range (mass fraction) is as
follows. manganese content of potentiometric titration ≥ 15.00%; manganese
content of ammonium iron (II) sulphate titrimetric method is 8.00% ~ 60.00%.
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 6682 Water for analytical laboratory use - Specification and test
methods
3 Method 1.Potentiometric titration
3.1 Principle
The sample is decomposed with hydrochloric acid, nitric acid, perchloric acid
and hydrofluoric acid, the insoluble residue is separated by filtration, the filtrate
is retained as a main solution. The filter paper containing the residue is burned,
the residue is melted with sodium carbonate. The melt is leached with
hydrochloric acid and combined with the main solution.
3.2 Reagents and materials
During the analysis, only approved analytical reagents and waters of grade 3
and above purity in accordance with GB/T 6682 are used.
3.2.1 Anhydrous sodium carbonate, solid.
3.2.2 Hydrochloric acid, ρ = 1.19 g/mL.
3.2.3 Hydrofluoric acid, ρ = 1.14 g/mL.
3.2.4 Perchloric acid, ρ = 1.67 g/mL.
3.2.5 Nitric acid, ρ = 1.42 g/mL.
3.2.6 Sulfuric acid, 1+1.
3.2.7 Hydrochloric acid, 1+4.
3.2.8 Sodium carbonate solution, 50 g/L.
3.2.9 Sodium pyrophosphate (Na2P2O7 • 10H2O) solution, 120 g/L. It is prepared
24 hours before use.
3.2.10 Filter type crucible, No.3.
3.5 Analytical procedures
3.5.1 Number of analyses
PERFORM at least two reproducibility analyses on the same sample.
3.5.2 Sample quantity
WEIGH 1.00 g of air-dried sample to the nearest 0.0001 g. WEIGH the
specimen in accordance with GB/T 14949.8 to determine the wet moisture
content.
3.5.3 Blank test
PERFORM blank test along with the sample.
3.5.4 Determination
3.5.4.1 Decomposition of samples
PLACE the sample (see 3.5.2) in a 300 mL Teflon beaker, ADD a few drops of
water to wet it, ADD 20 mL of hydrochloric acid (see 3.2.2) and 2 mL ~ 3 mL of
nitric acid (see 3.2.5), HEAT the solution to drive off the nitrogen oxidation.
3.5.4.2 Residue treatment
TRANSFER the filter paper containing the residue into a platinum crucible, DRY
it, ASH it, BURN it at 600 °C ~ 700 °C, ADD 2 g of sodium carbonate (see 3.2.1),
MELT it at 900 °C ~ 1000 °C. REMOVE the crucible and COOL it down.
3.5.4.3 Potentiometric titration
PIPETTE 100 mL of the solution into a 500 mL beaker containing 250 mL of
sodium pyrophosphate solution (see 3.2.9), CONTINUE stirring whilst adding
[if there is a precipitate, USE less solution or INCREASE the sodium
pyrophosphate solution (see 3.2.9), to ensure that the solution is clear].
3.2.13) to titrate it, until the potentiometric titrator (see 3.3.2) has obvious
potential sharp change or pointer deflection, as the end point.
3.6 Calculation of results
Calculate the manganese content (mass fraction) in the sample in accordance
with formula (3) or formula (4), expressed in %.
3.7 Allowable difference
The difference in analysis results shall not be greater than the allowable
difference listed in Table 1.
4 Method 2.ammonium iron (II) sulphate titrimetric method
4.1 Principle
After the sample is dissolved by hydrochloric acid, nitric acid and phosphoric
acid, in the phosphoric acid medium, ammonium phosphate or perchloric acid
is added to oxidize manganese to trivalent, the N-benzo anthranilic acid is used
as an indicator, use ammonium iron (II) sulphate standard titration solution to
titrate it.
4.2 Reagents and materials
During the analysis, only approved analytical reagents and waters of grade 3
and above purity in accordance with GB/T 6682 are used.
4.2.1 Ammonium nitrate, solid.
4.2.6 Sulfuric acid, 1 + 1.
4.2.7 Sulfuric acid, 5 + 95.
4.2.8 Sulfuric acid, 1 + 4.
4.2.9 Potassium dichromate standard solution [c (1/6 K2Cr2O7) = 0.04000 mol/L].
WEIGH 1.9615 g of reference potassium dichromate (pre-dried at 150 °C for 2
h and cooled to room temperature in a desiccator),
4.2.10.1 Preparation
WEIGH 15.68 g of ammonium iron (II) sulphate, DISSOLVE it in 1000 mL of
sulfuric acid (5 + 95) solution, MIX it uniformly.
4.2.10.2 Calibration
PIPETTE 25.00 mL of potassium dichromate standard solution (see 4.2.9) into
a 250 mL conical flask, ADD 40 mL of sulfuric acid (see 4.2.8) and 5 mL of
phosphoric acid (see 4.2.2), USE the ammonium iron (II) sulphate standard
titration solution (see 4.2.10) to titrate it until the orange color disappears, ADD
2 drops of the N-benzoanthranilic acid indicator solution (see 4.2.11),
CONTINUE adding it until the solution becomes green, which is the end point.
CALCULATE the titer T3 of manganese in the ammonium iron (II) sulphate
standard titration solution in accordance with formula (5), in grams per milliliter
(g/mL).
4.2.10.3 Determination of blank values
PIPETTE 10.00 mL of potassium dichromate standard solution (see 4.2.9) into
a 250 mL conical flask, ADD 40 mL of sulfuric acid (see 4.2.8) and 5 mL of
phosphoric acid (see 4.2.2), USE the ammonium iron (II) sulphate standard
titration solution (see 4.2.10) to titrate it until the orange color disappears.
4.2.11 N-benzoanthranilic acid indicator solution, 0.2 g/L. WEIGH 0.2 g of N-
benzoanthranilic acid, DISSOLVE it in a small amount of water, ADD 0.2 g of
sodium carbonate, HEAT to dissolve it at low temperature, ADD water to the
volume of 1000 mL, MIX it uniformly.
4.3 Instruments
The common laboratory instruments used in the analysis.
4.4 Sampling and preparation
PERFORM sampling and preparation in accordance with the provisions of GB/T
2011, the sample size shall be no more than 0.080 mm.
4.5 Analytical procedures
4.5.1 Number of analyses
PERFORM at least two repeatability analyses on the same sample.
4.5.3 Blank test
PERFORM the blank test along with the sample, MAKE titration in accordance
with 4.2.10.3, DO not add sulfuric acid and phosphoric acid, RECORD V12.
4.5.4 Determination
4.5.4.1.2 Perchloric acid oxidation
ADD 5 mL of hydrochloric acid (see 4.2.4), SHAKE it uniformly. ADD 20 mL of
phosphoric acid (see 4.2.2), SHAKE it uniformly. Then HEAT to dissolve it to
slight boiling, ADD 5 mL of nitric acid (see 4.2.3) while it is hot, SHAKE it in the
process of addition, after addition, SHAKE the conical flask sufficiently to
destroy the carbon and organic matter, HEAT it to the occurrence of slight
phosphoric acid smoke (the liquid level is calm). TAKE it off, ADD 2 mL of
perchloric acid (see 4.2.5), SHAKE it in the process of addition, HEAT it until
the solution level is calm to completely oxidize the divalent manganese, TAKE
it off.
4.5.4.2 COOL the solution obtained in 4.5.4.1.1 or 4.5.4.1.2 to about 70 °C,
ADD 50 mL of water, SHAKE it in the process of addition, after addition, SHAKE
it completely to dissolve the salt, USE flowing water to cool it to room
temperature. USE the ammonium iron (II) sulphate standard titration solution
(see 4.2.10) to titrate it to light red, ADD 2 drops of N-benzoanthranilic acid
indicator solution (see 4.2.11), CONTINUE titration until it becomes bright
yellow, which is the end point, RECORD V13.
4.6 Calculation of analysis results
4.6.1 Calculation of manganese content
CALCULATE the manganese content (mass fraction) wMn in the specimen in
accordance with formula (6), expressed in %.
5 General processing of analysis results
5.1 Acceptance of standard sample analysis values
When analyzing the sample, it is necessary to carry out the analysis of the same
standard sample along with the sample. The analytical value of the standard
sample shall meet the conditions of formula (7).
5.2 Calculation of final results
The final result is the arithmetic mean of the acceptable values of the specimen,
or the analytical value of the sample obtained in accordance with the procedure
specified in Appendix A. The numerical rounding off is carried out in accordance
with the provisions of GB/T 8170, the result retains two decimal places.
6 Test report
The test report shall include the following.
Appendix A
(Normative)
Specimen analysis value acceptance procedure flow chart
The flow chart of the sample analysis value acceptance procedure is shown in
Figure A.1.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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