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Analytical methods of anhydrous potassium fluoride
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GB/T 27813-2011: Analytical methods of anhydrous potassium fluoride---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/GBT27813-2011
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.060.01
G 10
Analytical methods of anhydrous potassium fluoride
Issued on: DECEMBER 30, 2011
Implemented on: JUNE 01, 2012
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... 4
2 Normative references... 4
3 Safety tips... 4
4 General... 5
5 Determination of potassium fluoride content... 5
6 Determination of chloride content... 6
7 Determination of loss on ignition... 8
8 Determination of free acid or free base content... 9
9 Determination of sulfate content... 10
10 Determination of fluorosilicate content... 12
11 Determination of water-insoluble matter content... 14
12 Determination of arsenic, iron, lead, chromium, silicon, boron, calcium and nickel
content... 15
Annex A (normative) Pretreatment and regeneration of H-732 ion exchange resin... 18
Analytical methods of anhydrous potassium fluoride
WARNING -- Personnel using this Standard should have practical experience in formal
laboratory work. This standard does not address all possible safety issues. Users are
responsible for taking appropriate safety and health measures and ensuring compliance
with the conditions stipulated in relevant national laws and regulations.
1 Scope
This Standard specifies the analytical methods for potassium fluoride content and
various impurities in anhydrous potassium fluoride.
This Standard applies to anhydrous potassium fluoride products.
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 6682-2008, Water for analytical laboratory use -- Specification and test
methods
HG/T 3696.1, Inorganic chemicals for industrial use -- Preparations of standard and
reagent solutions for chemical analysis -- Part 1.Preparations of standard
volumetric solutions
HG/T 3696.2, Inorganic chemicals for industrial use. Preparations of standard and
reagent solutions for chemical analysis. Part 2.Preparations of standard solutions
for impurity
HG/T 3696.3, Inorganic chemicals for industrial use. Preparations of standard and
reagent solutions for chemical analysis. Part 3.Preparations of reagent solutions
3 Safety tips
Some of the reagents used in this analytical method are toxic or corrosive. Exercise
caution when handling. If splashed on skin, rinse immediately with water. In severe
cases, seek medical attention immediately. Potassium fluoride is inherently toxic and
highly corrosive. Exercise caution when handling and wear protective equipment.
4 General
Unless otherwise specified, the reagents and water used in this Standard refer to
analytically pure reagents and Grade three water as specified in GB/T 6682-2008.The
standard titration solutions, impurity standard solutions, preparations, and products
used in the tests, unless otherwise specified, are prepared in accordance with HG/T
3696.1, HG/T 3696.2, and HG/T 3696.3.
5 Determination of potassium fluoride content
5.1 Method summary
Dissolve the test material in water. Exchange the solution with a strong acid cation
exchange resin to generate hydrofluoric acid. Titrate with a standard sodium hydroxide
solution using phenolphthalein as an indicator to obtain the result.
5.2 Reagents and materials
5.2.1 Sodium hydroxide standard titration solution. c(NaOH) ≈ 0.5 mol/L.
5.2.2 Phenolphthalein indicator solution. 10 g/L.
5.2.3 Asbestos.
5.2.4 H-732 ion exchange resin.
5.2.5 Carbon dioxide-free water.
5.3 Instruments and equipment
5.3.1 Ion exchange column. polyethylene plastic tube; inner diameter is 25 mm; length
is 500 mm; capable of controlling flow rate.
5.3.2 Plastic beaker.
5.4 Analysis procedure
5.4.1 Preparation of ion exchange column
Secure the ion exchange column to the stand. Close the stopcock. Fill the bottom of the
column with 1 cm thick asbestos. Pour approximately 10 mL of water into the column
to moisten it. Pour pretreated H-732 ion exchange resin into the column to a resin bed
height of 400 mm. Before use, treat the column according to the instructions in Annex
A.
5.4.2 Determination
Weigh approximately 1 g of specimen to the nearest 0.0002 g. Place in a 100 mL plastic
beaker. Dissolve in 50 mL of CO2-free water and inject into the ion exchange column.
Use CO2-free water as the eluent. Control the column flow rate to 5.0 mL/min~6.0
mL/min. Wash until the effluent is neutral (check with pH paper). Collect the effluent
in a 500 mL plastic beaker. Add 2 drops of phenolphthalein indicator solution. Titrate
with sodium hydroxide standard titrant until the solution turns pink and remains so for
30 s.
5.5 Result calculation
The potassium fluoride content is calculated as the mass fraction w1 of potassium
fluoride (KF) according to formula (1).
Where,
V - The volume of the sodium hydroxide standard titrant consumed during the titration,
in milliliters (mL);
c - The exact concentration of the sodium hydroxide standard titrant, in moles per liter
(mol/L);
m - The mass of the test material, in grams (g);
w2 - The mass fraction of chloride measured in Chapter 6;
1.639 - The conversion factor for chlorine to potassium fluoride;
w4 - The mass fraction of free acid measured in Chapter 8;
2.904 - The conversion factor for hydrofluoric acid to potassium fluoride;
w6 - The mass fraction of sulfate measured in Chapter 9;
1.210 - The conversion factor for sulfate to potassium fluoride;
M - The molar mass of potassium fluoride (KF), in grams per mole (g/mol) (M = 58.10).
The arithmetic mean of the parallel determination results is taken as the determination
result. The absolute difference between the two parallel determination results shall not
exceed 0.2%.
6 Determination of chloride content
6.1 Method summary
milliliters (mL);
V0 - The volume of the silver nitrate standard titrant consumed during the blank test, in
milliliters (mL);
c - The exact concentration of the silver nitrate standard titrant, in moles per liter
(mol/L);
m - The mass of the test material, in grams (g);
M - The molar mass of chlorine (Cl), in grams per mole (g/mol) (M = 35.45).
The arithmetic mean of the parallel determination results is taken as the determination
result. The absolute difference between the two parallel determination results shall not
exceed 0.01%.
7 Determination of loss on ignition
7.1 Apparatus and equipment
7.1.1 Platinum crucible.
7.1.2 High-temperature furnace. the temperature can be controlled within 650°C ± 20°C.
7.2 Analysis steps
Weigh approximately 5 g of specimen to the nearest 0.0002 g in a platinum crucible
that has been calcined at 650°C ± 20°C to a constant mass. Place the crucible in a high-
temperature furnace at 650°C ± 20°C for 2 h, remove it, and weigh it after cooling.
7.3 Result calculation
The loss on ignition is calculated as mass fraction w3 according to formula (3).
Where,
m1 - The mass of the test material and crucible before ignition, in grams (g);
m2 - The mass of the test material and crucible after ignition, in grams (g);
m - The mass of the test material, in grams (g).
The arithmetic mean of the parallel determination results is taken as the determination
result. The absolute difference between the two parallel determination results shall not
exceed 0.05%.
8 Determination of free acid or free base content
8.1 Reagents and materials
8.1.1 Sodium hydroxide standard titration solution. c(NaOH) ≈ 0.05 mol/L.
8.1.2 Hydrochloric acid standard titration solution. c(HCl) ≈ 0.05 mol/L.
8.1.3 Phenolphthalein indicator solution. 10 g/L.
8.1.4 Carbon dioxide-free water.
8.2 Apparatus
8.2.1 Plastic beaker.
8.2.2 Microburette. the graduation is 0.02 mL or 0.05 mL.
8.3 Analysis steps
Weigh approximately 5 g of specimen to the nearest 0.0002 g. Place in a 250 mL plastic
beaker. Dissolve in 50 mL of carbon dioxide-free water. Add 2 drops of phenolphthalein
indicator solution.
If the test solution is colorless, titrate with sodium hydroxide standard solution until the
solution turns pink and remains pink for 30 s.
If the test solution is red, titrate with standard hydrochloric acid solution until the
solution becomes colorless.
8.4 Result calculation
The free acid content is calculated as the mass fraction w4 of hydrofluoric acid (HF)
according to formula (4).
Where,
V - The volume of the sodium hydroxide standard titrant consumed during the titration,
in milliliters (mL);
c - The exact concentration of the sodium hydroxide standard titrant, in moles per liter
(mol/L);
m - The mass of the test material, in grams (g);
M - The molar mass of hydrofluoric acid (HF), in grams per mole (g/mol) (M = 20.01).
The free alkali content is calculated as the mass fraction w5 of potassium hydroxide
(KOH) according to formula (5).
Where,
V - The volume of the standard hydrochloric acid solution consumed during the titration,
in milliliters (mL);
c - The exact concentration of the standard hydrochloric acid solution, in moles per liter
(mol/L);
m - The mass of the test material, in grams (g);
M - The molar mass of potassium hydroxide (KOH), in grams per mole (g/mol) (M =
56.11).
The arithmetic mean of the parallel determination results is taken as the determination
result. The absolute difference between the two parallel determination results shall not
exceed 0.02%.
9 Determination of sulfate content
9.1 Method summary
The specimen is placed in a hydrochloric acid medium. Boric acid is added to complex
the fluoride ions. Then, an excess of barium chloride solution is added to precipitate the
sulfate ions into barium sulfate. Calculate the sulfate content based on the weight of the
barium sulfate.
9.2 Reagents
9.2.1 Boric acid.
9.2.2 Hydrochloric acid solution. 1 + 3.
9.2.3 Barium chloride solution. 100 g/L.
9.2.4 Methyl orange indicator solution. 1 g/L.
9.3 Instruments and equipment
0.4116 - The coefficient for converting barium sulfate to sulfate ions;
m - The mass of the test material, in grams (g).
The arithmetic mean of the parallel determination results is taken as the determination
result. The absolute difference between the two parallel determination results shall not
exceed 0.05%.
10 Determination of fluorosilicate content
10.1 Method summary
Fluoride ions in the specimen react with boric acid to form. Silicic acid reacts
quantitatively with ammonium molybdate in a slightly acidic solution to form
silicomolybdate heteropolyacid (silicomolybdate yellow). Adding a reducing agent
reduces silicomolybdate yellow to silicomolybdate blue. Measure the color at 795 nm
using a spectrophotometer or UV-visible spectrophotometer.
10.2 Reagents
10.2.1 Boric acid solution. 40 g/L.
10.2.2 Sulfuric acid solution. 1 + 33.
10.2.3 Ammonium molybdate solution. 100 g/L (refresh if precipitation occurs).
10.2.4 Oxalic acid solution. 50 g/L.
10.2.5 Stannous chloride hydrochloric acid solution. 20 g/L.
10.2.6 Silica standard solution. 1 mL of solution contains 0.01 mg of silicon dioxide
(SiO2).
Pipette 1.00 mL of the silica standard solution prepared according to HG/T 3696.2 into
a 100 mL volumetric flask. Dilute to the mark with water and shake well. Prepare this
solution immediately before use.
10.2.7 Saturated 2,4-dinitrophenol indicator solution.
10.3 Instrument
10.3.1 Spectrophotometer or UV-visible spectrophotometer. equipped with a 2 cm
cuvette.
10.3.2 Plastic beaker.
10.4 Analysis steps
result. The absolute difference between the two parallel determination results shall not
exceed 0.005%.
11 Determination of water-insoluble matter content
11.1 Method summary
Dissolve the specimen. Filter out the water-insoluble matter. Burn in a high-temperature
furnace until the mass remains constant. Calculate the water-insoluble matter content.
11.2 Reagents
Barium chloride solution. 100 g/L.
11.3 Instruments and equipment
11.3.1 Plastic beaker (polytetrafluoroethylene).
11.3.2 Plastic funnel.
11.3.3 High-temperature furnace. the temperature can be controlled within 500°C ±
20°C.
11.4 Analysis steps
Weigh approximately 30 g of specimen to the nearest 0.01 g. Place in a 250mL plastic
beaker. Add 100 mL of water and shake well. Heat the plastic beaker on a hot plate at
low temperature to completely dissolve the specimen. Filter through a plastic funnel
using slow-flow quantitative filter paper. Wash with water until fluoride ions are free
(test with barium chloride solution). Place the filter paper in a porcelain crucible that
has been calcined at 500℃ ±20℃ to a constant mass. Ash the crucible. Then calcine
the crucible in a high-temperature furnace at 500℃±20℃ until the mass is constant.
Remove the crucible. Cool and weigh.
11.5 Result calculation
The water-insoluble content is expressed as mass fraction w8 and is calculated
according to formula (8).
Where,
m1 - The mass of the porcelain crucible and water-insoluble substance, in grams (g);
m2 - The mass of the porcelain crucible, in grams (g);
m - The mass of the test material, in grams (g).
The arithmetic mean of the parallel determination results is taken as the determination
result. The absolute difference between the two parallel determination results shall not
exceed 0.05%.
12 Determination of arsenic, iron, lead, chromium, silicon, boron,
calcium and nickel content
12.1 Method summary
Inductively coupled plasma atomic emission spectrometry (ICP-AES) is used for
simultaneous determination of multiple elements.
12.2 Reagents
12.2.1 Nitric acid solution. 2+98 (guaranteed reagent).
12.2.2 Nitric acid solution. 1+10 (guaranteed reagent).
12.2.3 Mixed standard solution A. 1 mL of solution contains 0.02 mg each of arsenic
(As), iron (Fe), lead (Pb), chromium (Cr), boron (B), calcium (Ca), and nickel (Ni).
Pipette 2.00 mL of arsenic, iron, lead, chromium, boron, calcium, and nickel standard
solutions prepared according to HG/T 3696.2 into a 100 mL volumetric flask. Dilute to
the mark with nitric acid solution (12.2.1). Shake well. It shall be valid for 6~12 months.
12.2.4 Standard solution B. 1 mL of solution contains 0.05 mg of silicon (Si).
Pipette 5.00 mL of the silicon standard solution prepared according to HG/T 3696.2
into a 100 mL volumetric flask. Dilute to the mark with nitric acid solution (12.2.1).
Shake well. It shall be valid for 6~12 months.
12.2.5 Grade 1 water. comply with the requirements of GB/T 6682-2008.
12.3 Instruments and equipment
12.3.1 Inductively coupled plasma-atomic emission spectrometer (ICP-AES)
12.3.2 Fluorine-resistant torch
12.3.3 High-salt nebulizer
12.3.4 Plastic beaker (PTFE)
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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