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GB/T 3286.1-2012

Chinese Standard: 'GB/T 3286.1-2012'
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GB/T 3286.1-2012English160 Add to Cart 0--10 minutes. Auto immediate delivery. 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 Valid GB/T 3286.1-2012
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BASIC DATA
Standard ID GB/T 3286.1-2012 (GB/T3286.1-2012)
Description (Translated English) 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
Sector / Industry National Standard (Recommended)
Classification of Chinese Standard D52
Classification of International Standard 73.080
Word Count Estimation 18,132
Older Standard (superseded by this standard) GB/T 3286.1-1998
Quoted Standard GB/T 2007.2; GB/T 3286.2; GB/T 3286.3; GB/T 3286.4; GB/T 6379.2; GB/T 6682; GB/T 7728; GB/T 8170
Drafting Organization Wuhan Iron and Steel (Group)Corporation
Administrative Organization National Steel Standardization Technical Committee
Regulation (derived from) National Standards Bulletin 2012 No. 28
Proposing organization China Iron and Steel Association
Issuing agency(ies) General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China
Summary This standard specifies the complexometric titration of calcium oxide and magnesium oxide content and the use of atomic absorption spectrometry determination of magnesium oxide content. This section applies to limestone, dolomite calcium oxide and magnesi

GB/T 3286.1-2012
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
石灰石及白云石化学分析方法 第 1 部分: 氧化钙和氧化镁
含量的测定 络合滴定法和火焰原子吸收光谱法
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
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
WARNING: Personnel using this Part shall have formal laboratory work
experience. This Part does not point out all possible safety issues. It is
the responsibility of the user to take appropriate safety and health
measures and ensure compliance with the conditions specified by
relevant national laws and regulations.
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
titrate the combined content of calcium oxide and magnesium oxide; or mask
the calcium with slightly excessive EGTA standard titration solution, and use
cyclohexane diamine tetraacetic acid (CyDTA) standard titration solution to
titrate the magnesium oxide content.
For samples of which the iron oxide and alumina content is greater than 2.0 %
or the manganese oxide content is greater than 0.10 %, use sodium
diethylamine dithioformate (copper reagent) to precipitate and separate iron,
aluminum and manganese ions, and take the filtrate to titrate the calcium oxide
content and magnesium oxide content with EDTA or EGTA and CyDTA standard
titration solutions.
3.2 Reagents
Unless otherwise specified in the analysis, only approved analytical reagents
and distilled water of grade 3 or higher or water of equivalent purity that meets
the requirements of GB/T 6682 shall be used.
3.2.1 Mixed flux: TAKE two portions of anhydrous sodium carbonate and one
portion of boric acid, MIX well.
3.2.2 Hydrochloric acid (1 + 5).
3.2.3 Triethanolamine (1 + 4).
3.2.4 Ammonia water (1 + 1).
3.2.5 Potassium hydroxide solution (200 g/L), stored in plastic bottles. After
preparation, it shall be placed for more than 12 h before use.
3.2.6 Sodium diethylamine dithioformate (copper reagent) solution (50 g/L).
3.2.7 Ammonia buffer solution (pH10): WEIGH 67.5 g of ammonium chloride
and DISSOLVE in water, ADD 570 mL of ammonia water (ρ = 0.90 g/mL),
DILUTE to 1 L with water, MIX well.
3.2.8 Calcium indicator (calcium carboxylic acid): TAKE 1 g of calcium indicator
and GRIND with 100 g of sodium chloride, MIX well.
3.2.9 Acid chrome blue K-naphthol green B mixed indicator solution: TAKE 0.5
g of acid chrome blue K and 0.2 g of naphthol green B, DISSOLVE in water,
DILUTE to 70 mL with water.
NOTE: The ratio of acid chrome blue K and naphthol green B can be appropriately adjusted
according to the color development sensitivity of the indicator and the color discrimination ability
of the operator.
(mL);
V2 - the average value of the volume of EDTA standard titration solution
consumed in the titration, in milliliters (mL);
V02 - the average value of the volume of EDTA standard titration solution
consumed by the titration reagent blank, in milliliters (mL).
3.2.13 EGTA (ethylene glycol tetraacetic acid) standard titration solution
[c(EGTA) = 0.01 mol/L]
3.2.13.1 Preparation
WEIGH 3.90 g of EGTA, PLACE it in a 500 mL beaker, ADD about 250 mL of
water, HEAT at low temperature, dropwise ADD potassium hydroxide solution
(3.2.5) under constant stirring until the reagent is dissolved, and COOL to room
temperature. TRANSFER to a 1000 mL volumetric flask, DILUTE with water to
the mark, and MIX well.
3.2.13.2 Calibration of the titer of EGTA standard titration solution to
calcium oxide
Same as the calibration of the tire of EDTA standard titration solution to calcium
oxide. OPERATE according to 3.2.12.2 and CALCULATE the titer T3. USE
EGTA standard titration solution (3.2.13.1) instead of EDTA standard titration
solution (3.2.12.1).
3.2.14 CyDTA (cyclohexane diamine tetraacetic acid) standard titration
solution [c(CyDTA) = 0.01 mol/L]
3.2.14.1 Preparation
WEIGH 3.70 g of CyDTA, PLACE it in a 500 mL beaker, ADD about 250 mL of
water, HEAT at low temperature, dropwise ADD potassium hydroxide solution
(3.2.5) under constant stirring until the reagent is dissolved, and COOL to room
temperature. TRANSFER to a 1000 mL volumetric flask, DILUTE with water to
the mark, and MIX well.
3.2.14.2 Calibration of the titer of CyDTA standard titration solution to
magnesium oxide
Same as the calibration of the tire of EDTA standard titration solution to
magnesium oxide. OPERATE according to 3.2.12.3 and CALCULATE the titer
T4. USE CyDTA standard titration solution (3.2.14.1) instead of EDTA standard
titration solution (3.2.12.1).
3.3 Instruments
NOTE: This test solution can be used as a stock solution for the determination of calcium oxide,
magnesium oxide, silicon dioxide, aluminum oxide and iron oxide. It can be used for GB/T
3286.1 the determination of calcium oxide and magnesium oxide content by complexometric
titration method, GB/T 3286.2 the determination of silicon dioxide content by silicomolybdic blue
spectrophotometric method, GB/T 3286.3 the determination of aluminium oxide content by
chrome azurol S spectrophotometric method, GB/T 3286.4 the determination of iron oxide
content by o-phenanthroline spectrophotometric method. If the content of these chemical
components in the sample are determined at the same time, it may prepare only one portion of
stock solution of the sample, and then the stock solution is divided for the determination
according to each analysis method.
3.5.4.3 TAKE two portions of 25.00 mL of stock solution (3.5.4.2) (it may take
two portions of 15.00 mL for metallurgical lime samples), PLACE them in 250
mL or 500 mL Erlenmeyer flasks respectively, ADD 25 mL of water.
DETERMINE the calcium oxide content and magnesium oxide content by the
method specified in 3.5.5 or 3.5.6.
3.5.4.4 When the alumina and iron oxide content in the sample is greater than
2.0 % or the manganese oxide content is greater than 0.10 %, use copper
reagent to separate them: TAKE 100.00 mL of stock solution (3.5.4.2) into a
250 mL volumetric flask, ADD 50 mL of water, PUT a small piece of Congo red
test paper into the solution, NEUTRALIZE most of the acid with potassium
hydroxide solution (3.2.5), RINSE the bottleneck with water, dropwise ADD
ammonia water (3.2.4) to neutralize until the test paper is red, ADD 10 mL of
copper reagent solution (3.2.6), SHAKE vigorously for 1 min, COOL to room
temperature, DILUTE to the mark with water, MIX well, LEAVE for 30 min. DRY
filtrate with medium-speed quantitative filter paper, DISCARD the first 20 mL of
filtrate. TAKE two portions of 50.00 mL of filtrate, PLACE them in 250 mL
Erlenmeyer flasks respectively. DETERMINE the calcium oxide content and
magnesium oxide content by the method specified in 3.5.5 or 3.5.6.
3.5.5 Titration of calcium oxide content and magnesium oxide content
with EDTA
3.5.5.1 Titration of calcium oxide content
3.5.5.1.1 Limestone, metallurgical lime samples
In a portion of test solution (3.5.4.3 or 3.5.4.4), ADD 5 mL of triethanolamine
(3.2.3), MIX well, ADD 20 mL of potassium hydroxide solution (3.2.5) and about
0.1 g of calcium indicator (3.2.8), MIX well. TITRATE with EDTA standard
titration solution (3.2.12) until the test solution changes from red to bright blue,
which is the end point. For blank test and samples containing less than 1.0 %
magnesium oxide content, ADD 1.0 mL of magnesium oxide standard solution
(3.2.11) before titration with EDTA standard titration solution.
3.5.6.1.2 Dolomite samples
In a portion of test solution (3.5.4.3 or 3.5.4.4), ADD 5 mL of triethanolamine
(3.2.3), MIX well, ADD EGTA standard titration solution equivalent to 90 % to
95 % calcium oxide content in the titration solution (3.2.12), ADD 20 mL of
potassium hydroxide solution (3.2.5) and about 0.1 g of calcium indicator (3.2.8),
MIX well. Continue to TITRATE with EGTA standard titration solution (3.2.12)
until the test solution changes from red to bright blue, which is the end point.
Before the blank test titration, ADD 1.0 mL of magnesium oxide standard
solution (3.2.11), no titrant is preset.
NOTE: Same as the note of 3.5.5.1.2.
3.5.6.2 Titration of magnesium oxide
In another portion of test solution (3.5.4.3 or 3.5.4.4), ADD 5 mL of
triethanolamine (3.2.3), MIX well, ADD EGTA standard titration solution (3.2.13),
of which the added amount is 0.4 mL more than the volume of EGTA standard
titration solution consumed when titrating calcium oxide. ADD 20 mL of
ammonia buffer solution (3.2.7), ADD 4 to 5 drops of acid chrome blue K-
naphthol green B mixed indicator solution (3.2.9), TITRATE with CyDTA
standard titration solution (3.2.14) until the test solution changed from dark red
to blue green, which is the end point.
3.6 Calculation and representation of analysis results
3.6.1 Calculation of analysis results
3.6.1.1 Titration of calcium oxide content and magnesium oxide content
with EDTA
3.6.1.1.1 CALCULATE the mass fraction of calcium oxide according to formula
(3):
where:
w(CaO) - the mass fraction of calcium oxide;
V3 - the volume of EDTA standard titration solution consumed in the titration
of calcium oxide, in milliliters (mL);
V03 - the volume of EDTA standard titration solution consumed in the titration
of blank test solution, in milliliters (mL);
V05 - the volume of EGTA standard titration solution consumed in the titration
of blank test solution, in milliliters (mL);
T1 - the titer of EGTA standard titration solution to calcium oxide, in grams
per milliliter (g/mL);
m - the sample amount corresponding to the taken test solution, in grams (g).
3.6.1.2.2 CALCULATE the mass fraction of magnesium oxide according to
formula (6):
where:
w(MgO) - the mass fraction of magnesium oxide;
V6 - the volume of CyDTA standard titration solution consumed in the titration
of magnesium oxide, in milliliters (mL);
V03 - the volume of CyDTA standard titration solution consumed in the
titration of blank test solution, in milliliters (mL);
T4 - the titer of CyDTA standard titration solution to magnesium oxide, in
grams per milliliter (g/mL);
m - the sample amount corresponding to the taken test solution, in grams (g).
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. 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.
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. The joint test data is statistically
than 5 %;
Under reproducibility conditions, the absolute value of the difference between
the two independent analysis results obtained is not greater than the
reproducibility limit R, and the probability of exceeding the reproducibility limit
R is not greater than 5 %. For metallurgical lime samples, the interlaboratory
reproducibility limit is not required.
The raw data of the precision joint test are shown in Table B.2 and Table B.4.
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).
4.2.3 Perchloric acid (ρ = 1.67 g/mL).
4.2.4 Strontium chloride solution (60 g/L): TAKE 100 g of strontium chloride
(SrCl2 · 6H2O) in a 600 mL beaker, DISSOLVE it with water, TRANSFER it to a
1000 mL volumetric flask, DILUTE to the mark with water, MIX well.
4.2.5 Magnesium oxide standard solution
4.2.5.1 WEIGH 0.1000 g of high-purity magnesia (the content is not less than
99.99 %, it is burned at 950 °C ~ 1000 °C for 1 h and cooled to room
temperature in advance), PUT it in a 250mL beaker, ADD 10 mL of hydrochloric
acid (4.2.1) to dissolve, TRANSFER to a 1000 mL volumetric flask, DILUTE to
the mark with water, MIX well. 1.00 mL of this solution contains 100.0 μg of
magnesium oxide.
4.2.5.2 PIPETTE 50.00 mL of magnesium oxide standard solution (4.2.5.1) into
a 500 mL volumetric flask, ADD 10 mL of hydrochloric acid (4.2.1), DILUTE to
the mark with water, MIX well. 1.00 mL of this solution contains 10.0 μg of
magnesium oxide.
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.
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......
Related standard:   GB/T 3286.10-2020  GB/T 3286.5-2014
Related PDF sample:   GB/T 3286.8-2014
   
 
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