GB/T 5195.1-2017 PDF English
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| GB/T 5195.1-2017 | English | 210 |
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Fluorspar - Determination of calcium fluoride content - EDTA titration method and distillation-potentiometric titration method
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| GB/T 5195.1-2006 | English | 359 |
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Fluorspar -- Determination of calcium fluoride content
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| GB/T 5195.1-1985 | English | 199 |
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Methods for chemical analysis of fluor-spar--The EDTA volumetric method for the determination of calcium fluoride content
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GB/T 5195.1-2017: Fluorspar - Determination of calcium fluoride content - EDTA titration method and distillation-potentiometric titration 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/GBT5195.1-2017
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 73.080
D 52
Replacing GB/T 5195.1-2006
Fluorspar - Determination of calcium fluoride content -
EDTA titration method and distillation-potentiometric
titration method
Issued on. SEPTEMBER 07, 2017
Implemented on. JUNE 01, 2018
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine of PRC;
Standardization Administration of PRC.
Table of Contents
Foreword... 3
1 Scope... 5
2 Normative references... 5
3 EDTA titration method... 6
4 Distillation-potentiometric titration method... 13
5 Test report... 18
Appendix A (Informative) Joint test raw data... 19
Appendix B (Normative) Flowchart of acceptance procedure of specimen
analysis result... 20
Foreword
GB/T 5195 is divided into 16 parts.
- Part 1.EDTA titration method and distillation-potentiometric titration method;
- Part 2.Determination of carbonate content;
- Part 3.Determination of loss in mass at 105 °C - Gravimetric method;
- Part 4.Determination of sulfide content - Iodometric method;
- Part 5.Determination of total sulfur content - The iodometric method after
combustion;
- Part 6.Determination of phosphorus content - Photometric method;
- Part 7.Determination of zinc content - Flame atomic absorption
spectrophotometric method;
- Part 8.Determination of silicon dioxide content;
- Part 9.Determination of loss on ignition - Gravimetric method;
- Part 10.Determination of iron content - 1,10-phenanthroline
spectrophotometric method;
- Part 11.Determination of manganese content - The periodate
spectrophotometric method;
- Part 12.Determination of arsenic content - Atomic fluorescence
spectrometry;
- Part 13.Determination of aluminum content - EDTA titration method;
- Part 14.Determination of magnesium content - Flame atomic absorption
spectrometry;
- Part 15.Determination of calcium, aluminum, silicon, phosphorus, sulfur,
potassium, iron, barium and lead content - Wavelength dispersive X-ray
fluorescence spectrometric method;
- Part 16.Determination of silicon, aluminum, iron, potassium, magnesium
and titanium content - Inductively coupled plasma atomic emission
spectrometry.
This part is Part 1 of GB/T 5195.
This part was drafted in accordance with the rules given in GB/T 1.1-2009.
This part replaces GB/T 5195.1-2006 "Fluorspar - Determination of calcium
fluoride content". Compared with GB/T 5195.1-2006, the main technical
changes of this part are as follows.
- CHANGE the principle of the analysis method, from "When using EDTA
standard titration solution for titration to the disappearance of green
fluorescence, which is used as the end point; subtract the amount of
calcium carbonate in the sample, to calculate the mass fraction of calcium
fluoride in the sample" to "Take part of the filtrate under the condition of pH
greater than 12.5, use EDTA standard titration solution to titrate calcium, to
calculate the mass fraction of calcium fluoride” (see 3.1; 3.1 of the 2006
edition);
- MAKE corresponding changes on the relevant reagents and analytical
procedures (see 3.2 and 3.5; 3.2 and 3.4 of the 2006 edition);
- CARRY out a common test of precision between laboratories, using the
repeatability limit r and the reproducibility limit R obtained by statistics to
replace the "allowable error" (see 3.6.2 and 4.6.2; 3.6 and 4.7 in the 2006
edition);
- ADD the Appendix A "Raw data of common test" and Appendix B "Flowchart
of acceptance procedure of specimen analysis results” (see Appendix A and
Appendix B).
This part was proposed by the China Iron and Steel Industry Association.
This part shall be under the jurisdiction of the National Steel Standardization
Technical Committee (SAC/TC 183).
Drafting organizations of this part. Wuhan Iron and Steel (Group) Company,
Metallurgical Industry Information Standards Institute.
The main drafters of this part. Zhou Zheng, Wen Xiangdong, Chen Shihua,
Zhang Suizhong, Wu Lixin, Yang Yan, Zhang Jinying, Wen Bin, Zheng Feng,
Lu Chunsheng.
This part replaces the standard previously issued as follows.
- GB/T 5195.1-1985, GB/T 5195.1-2006.
Fluorspar - Determination of calcium fluoride content -
EDTA titration method and distillation-potentiometric
titration method
Warning - The personnel using this part shall have practical experience in
formal laboratory work. This part 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 part of GB/T 5195 specifies the methods for determining the content of
calcium fluoride by EDTA titration and distillation-potentiometric titration.
This part applies to the determination of calcium fluoride content in fluorite.
EDTA titration method has a measuring range (mass fraction). ≥ 60%;
distillation-potentiometric titration method has a measuring range (mass
fraction). ≥ 90%.
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 6379.1 Accuracy (trueness and precision) of measurement methods
and results - Part 1.General principles and definitions
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 8170 Rules of rounding off for numerical values & expression and
judgement of limiting values
3 EDTA titration method
3.1 Principle
The sample is leached with dilute acetic acid containing calcium, filtered,
decomposed by one of the following two methods.
3.2 Reagents
Unless otherwise specified in the analysis, only use approved analytical
reagents and distilled water of grade 3 or higher that meets the requirements of
GB/T 6682 or water of equivalent purity.
3.2.1 Sodium carbonate-boric acid mixed flux. take two parts of anhydrous
sodium carbonate and one part of boric acid; grind and mix it uniformly.
3.2.2 Hydroxylamine hydrochloride.
3.2.3 Absolute ethanol.
3.2.8 Potassium hydroxide solution, 200 g/L.
3.2.9 Magnesium sulfate solution, 5 g/L.
3.2.10 Triethanolamine, 1 + 2.
3.2.11 Calcium fluoride standard solution, 0.0015601 g/mL.
Weigh 1.0008 g of calcium carbonate ( > 99.99%) that has been pre-dried at
105 °C ~ 110 °C for 2 h and placed in a desiccator to cool to room temperature
in a 250 mL beaker; cover a watch glass; slowly add 25 mL of hydrochloric acid
(3.2.5). After the calcium carbonate is dissolved, add 100 mL of water; heat to
boil it; drive off the carbon dioxide; cool to room temperature. Transfer the
solution into a 500 mL volumetric flask; use water to dilute to the mark; mix it
uniformly. 1.00 mL of this calcium standard solution is equivalent to 0.0015601
g calcium fluoride.
3.2.13 Mix the indicator, weigh 0.20 g of calcein (C30H26N2O13), 0.12 g of
thymolphthalein (C28H30O4), and 20 g of anhydrous potassium sulfate in a
mortar; grind them fine and evenly; transfer to a suitable container; place it at
105 °C ± 5 °C to dry it for 1 h and cool it down. Store in a mouth-ground bottle
for later use.
3.4 Sample preparation
3.4.1 Prepare specimen according to GB/T 22564.
3.4.2 The specimen shall be processed to a particle size less than 0.063 mm,
dried at a temperature of 105 °C ± 5 °C for 2 h, placed in a desiccator to cool
to room temperature.
3.5 Analytical procedures
3.5.1 Number of determinations
For the same specimen (3.4.2), make at least 2 independent determinations.
3.5.2 Sample amount
Weigh 0.50 g of specimen, accurate to 0.0001 g.
3.5.3 Blank test
Do a blank test with the sample.
3.5.4 Sample decomposition
3.5.4.1 Alkali fusion
4 Distillation-potentiometric titration method
4.1 Principle
In the presence of perchloric acid, the fluorine in the sample is separated by
distillation with water vapor at 135 °C ± 2 °C through a temperature control
device; the distillate is absorbed by sodium hydroxide solution; the fluoride ion
selective electrode is used as the indicator electrode; the lanthanum nitrate
standard titration solution is used to titrate the amount of fluorine in the distillate,
to calculates the mass fraction of calcium fluoride.
4.2 Reagents
Unless otherwise specified in the analysis, only use approved analytical
reagents and distilled water of grade 3 or higher that meets the requirements of
GB/T 6682 or water of equivalent purity.
4.2.1 Potassium permanganate, crystalline.
4.2.3 Ethanol or isopropanol.
4.2.4 Perchloric acid, ρ = 1.67 g/mL.
4.2.5 Perchloric acid, 1 + 6.
4.2.6 Sodium hydroxide solution, 40 g/L, stored in a plastic bottle.
4.2.8 Buffer solution, pH 6.5.
Dissolve 140 g of hexamethylenetetramine in about 800 mL of water; use
perchloric acid (4.2.5) to neutralize to a pH of 6.5 ± 0.2; use water to dilute it to
1000 mL; if necessary, adjust the pH to 6.5.
4.2.9 Phenolphthalein solution, 5 g/L, prepared with 95% ethanol (volume
fraction).
4.3 Device
4.3.1 General laboratory equipment and gas generation and absorption devices.
4.3.2 The distillation device consists of a steam generator, a distillation flask, a
condenser tube, two electric heating jackets, a contact thermometer with a relay,
as shown in Figure 1, which can control the temperature of the distillation flask
to 135 °C ± 2 °C.
4.3.3 Magnetic stirrer.
4.3.4 pH meter, equipped with glass electrode and saturated calomel electrode.
4.3.5 Burette, 20 mL, graduation interval 0.02 mL.
4.3.6 Fluoride ion selective electrode.
4.3.7 Reference electrode, saturated calomel electrode or other types of
electrodes.
4.5.5 Potentiometric titration
Pipette 50.00 mL of test solution from a 500 mL volumetric flask in a 250 mL
beaker; add 10 mL of buffer solution (4.2.8) and 60 mL of ethanol (or
isopropanol) (4.2.3). Put the rotor of the magnetic stirrer into the beaker; place
the beaker on the stirrer; insert the fluorine ion selection electrode (4.3.6) and
the reference electrode (4.3.7); connect the potentiometer (4.3.8). Start the
magnetic stirrer; use lanthanum nitrate standard titration solution (4.2.7) to
titrate it; the titration speed is not more than 3.0 mL/min; record the volume of
the titration and the corresponding potential reading. When the potential change
speed increases, titrate at a slower speed. Determine the end point of the
titration from the drawn or recorded titration curve.
4.6 Calculation and presentation of results
4.7 Precision
The difference between two independent measurement results under
repeatability conditions is not greater than the repeatability limit r specified in
Table 2.
5 Test report
The test report shall include the following.
Appendix A
(Informative)
Joint test raw data
The precision data was determined in 2015 by 8 laboratories on 5 specimens
of different levels of calcium fluoride in fluorite. Each laboratory measures the
calcium fluoride content of each level independently three times under
repeatable conditions.
Appendix B
(Normative)
Flowchart of acceptance procedure of specimen analysis result
The flowchart of acceptance procedure of specimen analysis result is as shown
in Figure B.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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