NB/T 42006-2013 PDF English
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NB/T 42006-2013: Electrolyte for vanadium flow battery-teat 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/NBT42006-2013
NB
ENERGY INDUSTRY STANDARD OF
THE PEOPLE’S REPUBLIC OF CHINA
ICS 27.070
K 82
Record number. 41508-2013
Electrolyte for vanadium flow battery - test method
Issued on: JUNE 08, 2013
Implemented on: OCTOBER 01, 2013
Issued by. National Energy Administration
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative references... 4
3 Terms and definitions... 6
4 General requirements... 7
5 Sampling requirements... 8
6 Test methods... 8
Appendix A (Informative) Vanadium content test... 29
Appendix B (Informative) Vanadium content determination... 33
Electrolyte for vanadium flow battery - test method
1 Scope
This Standard specifies the terms and definitions, general requirements, sampling
requirements and test methods for electrolytes for vanadium flow battery, including the
determination methods of vanadium content, sulfate content, silicon content, iron
content, nitrogen content, other elements (K, Na, Al) content, conductivity, density and
viscosity.
This Standard applies to electrolytes for vanadium flow battery using sulfuric acid as a
solvent.
2 Normative references
The following documents are referred to in the text in such a way that some or all of
their content constitutes requirements of this document. For dated references, only the
dated version applies to this document. For undated references, the latest edition
(including all amendments) applies to this document.
GB/T 601-2002, Chemical reagent - Preparations of standard volumetric solutions
GB/T 602-2002, Chemical reagent - Preparations of standard solutions for impurity
GB/T 603-2002, Chemical reagent - Preparations of reagent solution for use in test
methods
GB/T 622-2006, Chemical reagent - Hydrochloric acid
GB/T 625-2007, Chemical reagent - Sulfuric acid
GB/T 626-2006, Chemical reagent - Nitric acid
GB/T 629-1997, Chemical reagent - Sodium hydroxide
GB/T 633-1994, Chemical reagent - Sodium nitrite
GB/T 639-2008, Chemical reagent - Sodium carbonate anhydrous
GB/T 643-2008, Chemical reagent - Potassium permanganate
GB/T 652-2003, Chemical reagent - Barium chloride dihydrate
GB/T 657-2011, Chemical reagent - Hexammonium heptamolybdate tetrahydrate
3 Terms and definitions
The following terms and definitions are applicable to this Standard.
3.1
vanadium flow battery, VFB
Also known as vanadium flow battery system, which is an energy storage device that
realizes the mutual conversion of electrical energy and chemical energy through the
electrochemical reaction of vanadium ions with different valence states in the positive
and negative electrolytes.
Note. A vanadium flow battery is mainly composed of power units (battery stacks
or battery modules), energy storage units (electrolyte and storage tanks),
electrolyte transport units (pipelines, valves, pumps, heat exchangers, etc.)
and battery management systems.
3.2
electrolyte
Solution – containing vanadium ions of different valence states – with ionic
conductivity.
3.3
electrolyte (3.5 valence)
When the molar concentration ratio of trivalent vanadium ions to tetravalent vanadium
ions in the electrolyte is 1.1, its valence state is defined as 3.5, and the electrolyte is
called electrolyte (3.5 valence).
3.4
positive electrolyte
The electrolyte when the battery is working has a different composition from the
electrolyte (3.5 valence) due to the change in the valence state of vanadium ions. The
positive electrolyte is the solution in the positive electrode storage tank of the battery,
which contains only tetravalent and pentavalent vanadium ions.
3.5
negative electrolyte
The electrolyte when the battery is working has a different composition from the
electrolyte (3.5 valence) due to the change in the valence state of vanadium ions. The
negative electrolyte is the solution in the negative electrode storage tank of the battery,
which contains only divalent and trivalent vanadium ions.
3.6
precipitation
The phenomenon that the active materials in the electrolyte accumulate or precipitate
and separate from the solution.
3.7
active material
The material that accepts and releases electrical energy during redox reactions during
the battery's bi-directional charging process.
Note. The active materials in the electrolyte for vanadium flow battery are
vanadium ions of different valence states.
4 General requirements
When performing electrolyte testing, the following general requirements shall be
followed.
a) Unless otherwise specified, the purity of reagents used in this Standard shall
be analytical reagents or above; the preparations and products used shall be
prepared in accordance with the provisions of GB/T 603-2002; the water for
laboratory use shall comply with the specifications of Grade 3 water in GB/T
6682-2008.
b) The concentrations of standard volumetric solutions prepared in this Standard
refer to the concentrations at room temperature. The analytical balance,
weights, burettes, volumetric flasks, pipettes, etc. used in the calibration, direct
preparation and use of standard volumetric solutions must be calibrated
regularly.
c) When calibrating and using standard volumetric solutions, the titration speed
shall generally be maintained at 1 mL/min ~ 3 mL/min.
d) Unless otherwise specified, standard volumetric solutions shall be stored at
room temperature (15 ℃ ~ 25 ℃) for no more than two months. If the solution
becomes turbid, precipitates, changes in color, etc., it shall be re-prepared.
e) All solutions expressed in percentage (%) in this Standard are mass fractions,
except for ethanol (95%) where the percentage (%) is volume fraction.
f) When testing with a cuvette in this Standard, ensure that the liquid to be tested
is between 1/3 and 2/3 of the cuvette.
5 Sampling requirements
When sampling and testing the electrolyte, the following requirements shall be
followed.
a) Before the products leave the factory, materials produced in one batch are
sampled as a batch.
b) The number of samples to be taken for each batch of products shall be
determined based on the uniformity of product mass.
c) Sampling shall be carried out in accordance with the requirements of 7.1.1.2
and 7.1.1.3 of GB/T 6680-2003.
6 Test methods
6.1 Appearance inspection
Visually inspect the color of the sample in a brightly lit room, where the color shall be
dark green with no precipitation inside.
Note. This Clause is specifically for electrolyte (3.5 valence).
6.2 Determination of vanadium content
6.2.1 Principle
Use sulfuric-phosphoric acid buffer solution as the medium; titrate with potassium
permanganate standard solution until a potential jump occurs; obtain the corresponding
electrolyte volume based on the potential jump; calculate the corresponding vanadium
ion concentration.
6.2.2 Reagents and solutions
The reagents used in the test shall meet the following requirements.
a) Potassium permanganate shall meet the requirements of GB/T 643-2008.
b) Sulfuric acid shall meet the requirements of GB/T 625-2007.
c) Phosphoric acid shall meet the requirements of GB/T 1282-1996.
d) Sodium oxalate shall meet the requirements of GB/T 1289-1994.
6.2.2.1 Preparation of solutions
The solutions used in the test shall be prepared as follows.
a) Sulfuric-phosphoric acid buffer solution. The volume fraction ratio is sulfuric
acid (50%). phosphoric acid (50%). water = 1.1.1.
b) Sulfuric acid solution (10%). Measure 57 mL of 98% concentrated sulfuric
acid into a beaker filled with water and dilute to 1 L.
c) Potassium permanganate. Standard solution of 𝑐ெைర = 0.015 mol/L. Weigh
2.370 0 g of potassium permanganate; dissolve it in 1 L of water; boil slowly
for 10 min ~ 15 min; place it in a dark place for one week; filter with a No. 4
glass filter pan; store in a brown bottle.
6.2.2.2 Calibration of potassium permanganate solution concentration
The calibration steps for potassium permanganate solution concentration are as follows.
a) Accurately weigh 1.000 0 g of standard sodium oxalate which has been dried
at 105℃ ~ 110℃ for 2 h and cooled to room temperature in a desiccator.
b) Dissolve the weighed standard sodium oxalate in 100 mL of sulfuric acid
solution (10%) and mix well.
c) Use the standard potassium permanganate solution prepared in 6.2.2.1 at 65 ℃
~ 70 ℃ for titration, until the solution turns pink and remains unchanged for
30 seconds; record the volume V1 of potassium permanganate solution
consumed at this time.
d) For a blank test, use the standard potassium permanganate solution prepared
in 6.2.2.1 at 65 ℃ ~ 70 ℃ to titrate 100 mL of sulfuric acid solution (10%),
until the solution turns pink and remains unchanged for 30 seconds; record the
volume V2 of potassium permanganate solution consumed at this time.
6.2.2.3 Result calculation
Calculate the concentration of the calibrated potassium permanganate solution
according to Formula (1).
Where.
𝑐ெைర – concentration of the calibrated potassium permanganate standard solution,
mol/L;
m – mass of sodium oxalate (accurate to 0.000 1 g), g;
M – molar mass of sodium oxalate, g/mol;
V1 – volume of potassium permanganate consumed by the calibration solution, mL;
V2 – volume of potassium permanganate consumed in the blank test, mL.
6.2.3 Test equipment
The instruments and accuracy used in the test shall meet the following requirements.
a) Potentiometric titrator. The potential accuracy is 0.1 mV.
b) Analytical balance. The accuracy is 0.000 1 g.
c) Other commonly used laboratory instruments.
6.2.4 Determination steps
6.2.4.1 Determination of electrolyte (3.5 valence)
The concentration of electrolyte (3.5 valence) is tested as follows.
a) Accurately pipette 0.2 mL of the test solution into a beaker containing 40 mL
of sulfuric-phosphoric acid buffer solution.
b) In a constant temperature water bath at 70 ℃, titrate potentiometrically until
two jump end points appear successively. According to the order of the time
when the jumps occur, the corresponding volumes of potassium permanganate
consumed are V3 and V4.
c) Calculate the corresponding vanadium concentration based on the volume of
potassium permanganate consumed at the end point of the jump.
6.2.4.2 Determination of negative electrolyte
The concentration of negative electrolyte is determined as follows.
a) Accurately pipette 0.2 mL of the test solution into a beaker containing 40 mL
of sulfuric-phosphoric acid buffer solution.
b) In a 70 ℃ constant temperature water bath, under the protection of argon,
perform potentiometric titration until three jump end points appear
successively. In the order of the time when the jumps occur, the corresponding
volumes of potassium permanganate consumed are V5, V6 and V7.
c) Calculate the corresponding vanadium concentration based on the volume of
potassium permanganate consumed at the end point of the jump.
6.4.2 Reagents and solutions
The reagents and solutions used in the test and their requirements are as follows.
a) Silicon dioxide.
b) Sodium carbonate. Shall comply with the requirements of GB/T 639-2008.
c) Oxalic acid. Shall comply with the requirements of GB/T 9854-2008.
d) Ascorbic acid. Shall comply with the requirements of GB/T 15347-1994.
e) Ammonium molybdate. Shall comply with the requirements of GB/T 657-
2011.5% solution, used after filtration.
f) Sulfuric acid-oxalic acid mixture. Weigh 50 g of oxalic acid; place it in a 2 000
mL beaker; add 500 mL of water; slowly add 200 mL of sulfuric acid; after it
dissolves, add 1 300 mL of water; mix well; cool to room temperature.
g) Ammonium ferrous sulfate. Shall comply with the requirements of GB/T 661-
2011.6% solution, 5 mL of sulfuric acid in 100 mL, used after filtration.
h) Ascorbic acid reducing agent (prepare before use). Weigh 4 g of ascorbic acid
and 0.2 g of ammonium ferrous sulfate; dissolve them in water and dilute to
100 mL; add a few drops of sulfuric acid (98%).
i) Silicon standard solution.
1) Silicone standard solution A. Weigh 1.070 0 g of pure silicon dioxide that
has been dried at 105 ℃ ~ 110 ℃ for 1 h and cooled to room temperature
in a desiccator; place it in a platinum crucible pre-filled with 6.000 0 g of
sodium carbonate (not containing silicon dioxide); stir well and cover with
a small amount of sodium carbonate; melt in a 900 ℃ high-temperature
furnace for 30 min; take out and cool; place in a 500 mL plastic beaker;
use boiling water to leach the molten block and dissolve it; take out the
crucible; use water to rinse the solute on it; use water to dilute the solution
in the beaker to the scale; shake well; store in a plastic bottle for later use.
1 mL of this solution contains 1 mg of silicon.
2) Silicon standard solution B (prepare before use). Pipette 10 mL of silicon
standard solution A into a 500 mL volumetric flask; use water to dilute to
the mark; shake well. Store in a dry plastic bottle. 1 mL of this solution
contains 0.02 mg of silicon.
6.4.3 Test equipment
The instruments and requirements used in the test are as follows.
a) Spectrophotometer. Its performance and operation shall conform to the
relevant provisions of GB/T 7729-1987.
b) Other commonly used laboratory instruments.
6.4.4 Determination steps
6.4.4.1 Drawing of standard curve
Follow the steps below to draw the standard curve.
a) Accurately pipette 0.00, 1.00, 2.00, 3.00, and 5.00 mL of silicon standard
solution B into 50 mL volumetric flasks, respectively.
b) Add 5 mL of ammonium molybdate solution respectively; use a small amount
of water to rinse the bottle mouth; shake well.
c) After standing for 15 ~ 20 minutes, add 10 mL of sulfuric acid-oxalic acid
mixture and quickly add 2 mL of ascorbic acid (4%).
d) Add water to dilute; fix the volume; shake well.
e) After 15 minutes, measure the absorbance at a wavelength of 660 nm using a
1 cm cuvette with the blank reagent as reference.
f) Draw a standard curve with the silicon content (in mg) as the abscissa and the
corresponding absorbance as the ordinate.
6.4.4.2 Sample determination
Follow the steps below to test the silicon content.
a) Use a pipette to transfer 2 mL of the sample to be tested into a 100 mL
volumetric flask; fix the volume; shake well.
b) Transfer 10 mL of the solution prepared in step a) into a 50 mL volumetric
flask.
c) Repeat steps b) ~ e) of 6.4.4.1.
d) Obtain the corresponding silicon content m on the standard curve according to
the measured absorbance.
6.4.5 Result calculation
The silicon content is calculated according to Formula (9).
Where.
cSi – content of silicon in the sample, mg/L;
m – silicon content obtained from the standard curve according to the sample
absorbance, mg;
V – sample volume, mL.
6.5 Determination of iron content
6.5.1 Principle
Directly absorb the sample to be tested and use sodium hydroxide to neutralize it; use
hydroxylamine hydrochloride to reduce the high-valent iron and eliminate the
interference of copper at the same time. In a solution with a pH value of 3 ~ 5, low-
valent iron reacts with o-phenanthroline to form an orange-red complex, which is
determined by spectrophotometry.
6.5.2 Reagents and solutions
The reagents and solutions used in the test and their requirements are as follows.
a) Hydroxylamine hydrochloride. Shall comply with the requirements of GB/T
6685-2007.10% solution.
b) Sodium hydroxide. Shall comply with the requirements of GB/T 629-1997.10%
solution.
c) 1,10-phenanthroline (o-phenanthroline). Shall comply with the requirements
of HG/T 4018-2008.0.1% solution.
d) Iron wire. The iron content shall be above 99.99%.
e) Sodium acetate. Shall comply with the requirements of GB/T 694-1995.
f) Acetic acid. Shall comply with the requirements of GB/T 676-2007.
g) Nitric acid. Shall comply with the requirements of GB/T 626-2006.
6.5.3 Solution preparation
The solutions and preparation steps used in the test are as follows.
a) Sodium acetate-acetic acid buffer solution. Weigh 4.000 0 g of sodium acetate
and dissolve it in an appropriate amount of water; add 27 mL of acetic acid
(36%); use water to dilute to 100 mL; mix well.
b) 0.1% o-phenanthroline solution. Weigh 0.100 0 g of o-phenanthroline and
place it in a small amount of water; add two drops of 1+1 hydrochloric acid;
dissolve it; use water to dilute it to 100 mL; store it in a brown bottle.
c) Iron standard solution. Solution A, 1 mL contains 0.1 mg of iron; Solution B,
1 mL contains 0.01 mg of iron.
1) Preparation method of solution A. Weigh 0.100 0 g of pure iron wire with
an iron content of more than 99.99% and place it in a 100 mL beaker; add
10 mL of 1+1 nitric acid and dissolve it under slight heat; use a small
amount of water to wash the wall of the beaker; heat to remove nitrogen
oxides; after cooling, transfer it to a 1 000 mL volumetric flask; use water
to dilute it; fix the volume; shake well.
2) Preparation method of solution B. When using, accurately pipette 10 mL
of Solution A; place it in a 100 mL volumetric flask; use water to dilute;
fix the volume; shake well.
6.5.4 Test equipment
The instruments and requirements used in the test are as follows.
a) Spectrophotometer. The operation shall comply with the relevant provisions of
GB/T 7729-1987.
b) Other commonly used laboratory instruments.
6.5.5 Determination steps
6.5.5.1 Drawing of standard curve
The standard curve is drawn according to the following steps.
a) Accurately pipette 0.00, 1.00, 2.00, 3.00, 5.00, and 6.00 mL of iron standard
solution B into 50 mL volumetric flasks, respectively.
b) Use water to dilute to about 25 mL; use sodium hydroxide (10%) to adjust the
pH to 3 ~ 5; shake well.
c) Add 5 mL of hydroxylamine hydrochloride (10%) solution, 5 mL of acetic
acid-sodium acetate buffer solution, and 5 mL of o-phenanthroline solution
(0.1%) in sequence.
d) Place at room temperature for 30 minutes; dilute to volume; shake well.
e) Measure the absorbance at a wavelength of 510 nm using the blank reagent as
a reference.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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