GB/T 3286.1-2012 PDF English                    
       
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			| GB/T 3286.1-2012 | English | 160 | 
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                    Methods for chemical analysis of limestone and dolomite - Part 1: The determination of calcium oxide and magnesium oxide content - The complexometric titration method and the flame atomic absorption spectrometric method
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			| GB/T 3286.1-1998 | English | 439 | 
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                    Methods for chemical analysis of limestone and dolomite--The determination of calcium oxide and magnesium oxide content
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			| GB/T 3286.1-1982 | English | RFQ | 
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                    Chemical analysis of limestone and dolomite--The EDTA-CYDTA volumetric method for determination of calcium oxide and magnesium oxide
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    GB/T 3286.1-2012: Methods for chemical analysis of limestone and dolomite - Part 1: The determination of calcium oxide and magnesium oxide content - The complexometric titration method and the flame atomic absorption spectrometric method
  ---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT3286.1-2012  
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 73.080
D 52
Replacing GB/T 3286.1-1998
Methods for chemical analysis of limestone and dolomite -
Part 1.The determination of calcium oxide and magnesium
oxide content - The complexometric titration method and the
flame atomic absorption spectrometric method
Issued on. NOVEMBER 05, 2012
Implemented on. MAY 01, 2013
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine of the People's Republic of China;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword... 3
1 Scope... 5
2 Normative references... 5
3 Complexometric titration method... 6
4 Flame atomic absorption spectrometric method... 18
5 Test report... 23
Annex A (normative) Flow chart of the acceptance procedure of sample
analysis results... 24
Annex B (informative) Function relationships and raw data of precision test. 25
1 Scope
This Part of GB/T 3286 specifies the determination of calcium oxide and
magnesium oxide content by complexometric titration method and the
determination of magnesium oxide content by atomic absorption spectrometric
method.
This Part applies to the determination of calcium oxide content and magnesium
oxide content in limestone and dolomite. It also applies to the determination of
calcium oxide content and magnesium oxide content in metallurgical lime.
Complexometric titration method, determination range (mass fraction). calcium
oxide content is greater than 20 %, magnesium oxide content is greater than
2.5 %; atomic absorption spectrometric method, determination range (mass
fraction). magnesium oxide content is 0.1 % ~ 2.5 %.
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 2007.2 General rules for the sampling and sample preparation of
minerals in bulk - Sample preparation by manual method
GB/T 3286.2 Methods for chemical analysis of limestone and dolomite - Part
2.The determination of silicon dioxide content - The silicomolybdic blue
spectrophotometric method and the perchloric acid dehydration gravimetric
method
GB/T 3286.3 Methods for chemical analysis of limestone and dolomite - Part
GB/T 6379.2 Accuracy (trueness and precision) of measurement methods
and results - Part 2.Basic method for the determination of repeatability and
reproducibility of a standard measurement method
GB/T 6682 Water for analytical laboratory use - Specification and test
methods
GB/T 7728 Chemical analysis of metallurgical products - General rule for
flame atomic absorption spectrometric methods
GB/T 8170 Rules of rounding off for numerical values & expression and
judgement of limiting values
3 Complexometric titration method
3.1 Principle
The sample is melted with sodium carbonate-boric acid mixed flux and leached
with dilute hydrochloric acid.
3.3 Instruments
Use common laboratory instruments and equipment.
3.4 Sample preparation
3.4.1 PREPARE samples according to GB/T 2007.2.
3.4.2 The samples shall be processed to a particle size of less than 0.125 mm.
3.4.3 Before analysis, limestone and dolomite samples are dried at 105 °C ~
110 °C for 2 h, and then placed in a desiccator to cool to room temperature.
3.4.4 The preparation of metallurgical lime samples shall be carried out quickly.
After the samples are made, they shall be immediately sealed in a ground-
mouth bottle or plastic bag and stored in a desiccator. The samples are not be
dried before analysis.
3.5 Analysis steps
3.6.2 Determination and representation of analysis results
If the absolute value of the difference between the two independent analysis
results of the same sample is not greater than the repeatability limit r value, the
arithmetic mean is taken as the analysis result.
3.7 Precision
The precision data is determined in 2011 by 8 laboratories on samples with 5
different levels of calcium oxide and magnesium oxide content. Each laboratory
independently determines the calcium oxide and magnesium oxide content
three times under repeatability conditions.
4 Flame atomic absorption spectrometric method
4.1 Principle
The sample is decomposed with hydrochloric acid and hydrofluoric acid.
Perchloric acid smokes and drives out the hydrofluoric acid. In the presence of
strontium chloride, the test solution is sprayed into an air-acetylene flame. A
magnesium hollow cathode lamp is used as the light source. The absorbance
is measured at a wavelength of 285.2 nm of an atomic absorption spectrometer.
4.2 Reagents
4.2.1 Hydrochloric acid (1 + 1).
4.2.2 Hydrofluoric acid (ρ = 1.13 g/mL).
4.2.5 Magnesium oxide standard solution
4.3 Instruments
Atomic absorption spectrometer, equipped with air-acetylene burner,
magnesium hollow cathode lamp. The air and acetylene gas must be
sufficiently pure (no water, oil, and magnesium) to provide a stable, clear flame.
CHECK the performance of the atomic absorption spectrometer according to
the requirements of GB/T 7728.The instruments used shall meet the following
indicators.
4.3.1 Minimum precision requirements
MEASURE the absorbance 10 times using the standard solution of the highest
concentration, and calculate the average value and standard deviation of the
absorbances. The standard deviation shall not exceed 1.0 % of the average
absorbance.
4.3.2 Characteristic concentration
The characteristic concentration of magnesium oxide shall be better than 0.007
μg/mL.
4.3.3 Detection limit
The detection limit of magnesium oxide shall be better than 0.004 μg/mL.
4.3.4 Linearity of the calibration curve
The calibration curve is divided into 5 sections according to the concentration.
The ratio of the difference between the absorbance difference in the highest
section and the difference in absorbance in the lowest section should not be
less than 0.7.
4.4 Sample preparation
4.5 Analysis steps
4.5.1 Determination times
For a same sample (4.4.3 or 4.4.4), determine at least 2 times independently.
4.5.2 Sample amount
WEIGH 0.20 g of sample, to the nearest 0.0001 g. For metallurgical lime
samples, the samples shall be quickly weighed.
4.5.3 Blank test
CARRY OUT the blank test along with the sample.
4.5.4 Sample decomposition and preparation of test solution
4.5.4.3 Test solution
4.5.4.3.1 PIPETTE 10.00 mL of test solution (4.5.4.2) into a 100 mL volumetric
flask, ADD 5 mL of hydrochloric acid (4.2.1) and 5.0 mL of strontium chloride
solution (4.2.4), DILUTE to the mark with water, MIX well. This test solution is
used for the determination of 0.1 % ~ 0.50 % of magnesium oxide content.
4.5.4.3.2 PIPETTE 20.00 mL of test solution (4.5.4.3.1) into a 100 mL
volumetric flask, ADD 5 mL of hydrochloric acid (4.2.1) and 5.0 mL of strontium
chloride solution (4.2.4), DILUTE to the mark with water, MIX well. This test
solution is used for the determination of more than 0.50 % of magnesium oxide
content.
4.5.6 Plotting of calibration curve
PIPETTE 0 mL, 1.00 mL, 2.00 mL, 4.00 mL, 6.00 mL, 8.00 mL, 10.00 mL of
magnesium oxide standard solution (4.2.5.2) respectively into a set of 100 mL
volumetric flasks, each ADD 5 mL of hydrochloric acid (4.2.1) and 5.0 mL of
strontium chloride solution (4.2.4), DILUTE to the mark with water, MIX well. At
a wavelength of 285.2 nm of the atomic absorption spectrometer, ADJUST the
zero point with water and measure the absorbance. PLOT the calibration curve
with the concentration of magnesium oxide as the abscissa and the absorbance
subtracting the zero-concentration solution as the ordinate.
4.6 Calculation and representation of analysis results
4.6.2 Determination and representation of analysis results
If the absolute value of the difference between the two independent analysis
results of the same sample is not greater than the repeatability limit r value, the
arithmetic mean is taken as the analysis result. If the absolute value of the
difference between the two independent analysis results is greater than the r
value, increase the number of measurements and determine the analysis result
as specified in Annex A.
The analysis result is rounded off according to GB/T 8170, and the numerical
value is rounded off to two decimal places.
4.7 Precision
The precision data is determined in 2011 by 8 laboratories on samples with 5
different levels of magnesium oxide contents. Each laboratory independently
determines the magnesium oxide contents three times under repeatability
conditions.
5 Test report
The test report shall include the following contents.
...... Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.  
      
    
     
    
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