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HG/T 3247-2017 (HG/T3247-2017)

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HG/T 3247-2017: PDF in English (HGT 3247-2017)
HG/T 3247-2017
HG
CHEMICAL INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 71.060.50
G 12
Record No.: 60522-2018
Replacing HG/T 3247-2008
Potassium Perchlorate for Industrial Use
工业高氯酸钾
ISSUED ON: NOVEMBER 07, 2017
IMPLEMENTED ON: APRIL 01, 2018
Issued by: Ministry of Industry and Information Technology of PRC
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Normative References ... 5
3 Molecular Formula and Relative Molecular Mass ... 6
4 Classification ... 6
5 Requirements ... 7
6 Test Methods ... 7
7 Inspection Rules ... 26
8 Markings and Labels ... 27
9 Packaging, Transportation and Storage ... 27
Potassium Perchlorate for Industrial Use
Warning: According to the provisions of Clause 6 in GB 12268-2012, this product
belongs to the oxidizing substances of item 5.1 in category 5. Care shall be taken
during operation. Personnel using this standard shall have practical experience
working in formal laboratory. This standard does not point out all possible safety
issues. It is the user's responsibility to take appropriate safety and health
measures and to ensure compliance with the conditions stipulated by relevant
national regulations.
1 Scope
This Standard specifies the requirements, test methods, inspection rules, marking,
labels, packaging, transportation, and storage of potassium perchlorate for industrial
use.
This Standard is applicable to potassium perchlorate for industrial. This product is
mainly used to manufacture fireworks and firecrackers, safety matches, meteorological
rockets, civil ignition coal, oxidants, and automobile airbags, etc.
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 document.
GB 190-2009 Packing Symbol of Dangerous Goods
GB/T 191-2008 Packaging - Pictorial Marking for Handling of Goods
GB/T 3051-2000 Inorganic Chemical Products for Industrial Use - General Method
for Determination of Chloride Content - Mercurimetric Method
GB/T 6003.1-2012 Test Sieves - Technical Requirements and Testing - Part 1: Test
Sieves of Metal Wire Cloth
GB/T 6678 General Principles for Sampling Chemical Products
GB/T 6682-2008 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
GB 10631-2013 Safety and Quality for Fireworks
GB 12268-2012 List of Dangerous Goods
GB 12463-2009 General Specifications for Transport Packages of Dangerous
Goods
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: Preparation of Reagent
Solutions
JJG 119-2005 Verification Regulation of Laboratory pH Meters
Provisions on the Administration of the Road Transport of Dangerous Goods
Rule for the Waterway Transport of Dangerous Goods
Provisions on Supervision and Administration of Transport Safety of Railway
Dangerous Goods
Interim Provisions on the Administration of Transport of Railway Dangerous Goods
3 Molecular Formula and Relative Molecular Mass
Molecular formula: KClO4
Relative molecular mass: 138.55 (according to 2016 international relative atomic mass)
4 Classification
Potassium perchlorate for Industrial use is divided into Type-I and Type-II; and its main
uses are as follows:
---Type-I products are mainly used for meteorological rocket propulsion, oxidants,
6.3.4.1 Preparation of test solution
Take about 1g pre-ground powder sample, accurate to 0.0002g. Place it in a nickel
crucible; add 6g of sodium nitrite ground into powder; and mix thoroughly. Cover it; put
in a high-temperature furnace; gradually raise the temperature to 500°C; melt at this
temperature for 1.5 h. Cool off; dissolve the melt by hot water and wash into the beaker.
Cool off and transfer all to a 250 mL (V1) volumetric flask; dilute to the mark by water;
and shake well.
6.3.4.2 Test
Pipette 50 mL (V2) of test solution into a 500mL conical flask; add 50mL of silver nitrate
standard titration solution and 15mL of nitric acid solution by a pipette; and heat to all
nitrogen dioxide gas escape. Cool off, add 5mL of nitrobenzene; and shake for 30s.
Add 5mL of ferric ammonium sulfate indicator solution and use potassium thiocyanate
standard titration solution to titrate until the solution appears red. Do a blank test at the
same time.
6.3.5 Test data processing
The content of potassium perchlorate is calculated by the mass fraction w1 of
potassium perchlorate (KCIO4), and is calculated according to Formula (1):
Where:
V0 - the volume of potassium thiocyanate standard titration solution consumed by
titration of blank solution, in mL;
V - the volume of potassium thiocyanate standard titration solution consumed by
titration of test solution, in mL;
c - Accurate value of the concentration of potassium thiocyanate standard titration
solution, in mol/L;
M - The value of the molar mass of potassium perchlorate (KClO4), in (g/mol)
(M=138.6);
m – value of mass of the sample, in g;
V1 – value of volume of test solution in 6.3.4.1, in mL;
V2 – value of volume of the transferred test solution in 6.3.4.2, in mL;
6.5 Determination of chloride content
6.5.1 Principle
According to Clause 3 of GB/T 3051-2000.
6.5.2 Reagents and materials
According to Clause 4 of GB/T 3051-2000.
6.5.3 Test procedures
Take about 10g of sample, accurate to 0.01g. Place it in a 250mL conical flask; add
100mL of water; and heat until the sample is completely dissolved. Cool off, add 2~3
drops of bromophenol blue indicator solution; titrate the nitric acid solution (1mol/L)
until it is just yellow, and then add 2~3 drops in excess. Add 1mL of phenylazoformic
acid 2-phenylhydrazide indicator solution; and titrate by mercury
nitrate standard titration solution until the solution turns from yellow to purple. Do a
blank test at the same time. The treatment of mercury-containing waste liquid shall be
carried out in accordance with Appendix D in GB/T 3051-2000.
6.5.4 Test data processing
The chloride content is calculated by the mass fraction w3 of potassium chloride (KCl),
and is calculated according to Formula (3):
Where:
V – value of volume of mercury nitrate standard titration solution consumed by titration
of test solution, in mL;
V0 – value of volume of mercury nitrate standard titration solution consumed by titration
of blank solution, in mL;
c – accurate value of the concentration of mercury nitrate standard titration solution, in
mol/L;
M – value of mole mass of chloride (by KCl), in (g/mol) (M=74.55);
m – value of mass of the sample, in g.
The arithmetic mean of the parallel determination results is taken as the determination
0.2mL, the adding amount of ferrous ammonium sulfate standard titration solution shall
be appropriately increased (accurately add by a pipette). Do a blank test at the same
time.
6.6.5 Test data processing
The content of chlorate is calculated by the mass fraction w4 of potassium chlorate
(KC1O3), and is calculated according to Formula (4):
Where:
V0 – value of volume of the potassium permanganate standard titration solution
consumed by titration of blank solution, in mL;
V - value of volume of the potassium permanganate standard titration solution
consumed by titration of test solution, in mL;
c – accurate value of the concentration of the potassium permanganate standard
titration solution, in mol/L;
M – value of mole mass of the potassium chlorate , in (g/mol) (M=20.42);
m – value of mass of the sample, in g.
The arithmetic mean of the parallel determination results is taken as the determination
result; and the absolute difference between the two parallel determination results shall
be no more than 0.003%.
6.7 Determination of hypochlorite content
6.7.1 Principle
The hypochlorite (ClO-) in the test solution may oxidize the iodide ion into iodine (I2);
and use starch-potassium iodide test paper to determine whether there is hypochlorite
in the sample. The main reaction formula is as follows:
6.7.2 Reagents and materials
Starch-potassium iodide test paper.
6.7.3 Test procedures
Where:
V – value of volume of the sodium thiosulfate standard titration solution consumed by
titration of test solution, in mL;
V0 – value of volume of the sodium thiosulfate standard titration solution consumed by
titration of blank solution, in mL;
c – accurate value of concentration of the sodium thiosulfate standard titration solution,
in mol/L;
M – value of mole mass of potassium bromate , in (g/mol) (M=27.83);
m – value of mass of the sample, in g.
The arithmetic mean of the parallel determination results is taken as the determination
result; and the absolute difference between the two parallel determination results shall
be no more than 0.002%.
6.9 Determination of sodium content
6.9.1 Principle
After the sample is dissolved in water, the sample is introduced into the flame; and the
sample is evaporated, dissociated, atomized, and excited to emit light by the thermal
and chemical effects of the flame (1800°C to 2500°C). According to the relationship
between the emission intensity i of the characteristic spectral line and the concentration
c of the measured element in the sample, that is, i = αcb (α and b are constants),
determine the sodium content in the sample.
6.9.2 Reagents or materials
6.9.2.1 Potassium standard solution: 1mL solution contains 1mg of potassium (K).
6.9.2.2 Sodium standard solution: 1mL solution contains 1mg of sodium (Na).
6.9.3 Apparatus
Flame spectrophotometer.
6.9.4 Test procedures
6.9.4.1 Drawing of working curve
6.10.1.3 Apparatus
Micro burette: division of 0.02mL.
6.10.1.4 Test procedures
Take about 5g of sample, accurate to 0.0002g. Place it in a 250mL beaker; add 100mL
of water; and heat to dissolve. Add 10mL of hydrochloric acid solution; and then make
it slightly alkaline with ammonia water. Boil the solution and filter if necessary. Adjust
to acidity with oxalic acid solution; then add 10 mL of excess oxalic acid solution; and
heat to boil. Add 10 mL of ammonium oxalate solution under rapid stirring; and keep
the pH value of the solution at 3.5~4.5 (check with accurate pH test paper). Keep warm
on boiling water bath for more than 1h. Cool to room temperature and filter by
quantitative filter paper. Wash the precipitate and filter paper by water and filter until
there is no oxalic acid (tested by resorcinol test method). Collect the washing solution
and filtrate and mix them together. This solution is Test Solution A and is used for the
determination of magnesium salt content. Dissolve the precipitate by 10 mL of sulfuric
acid solution (see 6.10.1.2.6) and thoroughly wash the filter paper by hot water.
Combine the filtrate and the washing solution in a 250mL conical flask; dilute with water
to about 100mL; heat to about 60°C; use potassium permanganate standard titration
solution to titrate the solution until the solution appears pink and does not fade within
15s.
NOTE: The resorcinol test method -- take 1mL of the filtrate; put it in a test tube; add 2~3 drops
of sulfuric acid solution (see 6.10.1.2.7) and a small amount of magnesium powder. When the
magnesium powder is completely dissolved, add about 0.1g of resorcinol and shake until
dissolved. After cooling, carefully add 3~4 drops of sulfuric acid along the tube wall. A blue ring
is formed at the interface of the two liquids. When the lower sulfuric acid is heated, the blue
color spreads downward from the interface, making the sulfuric acid layer blue.
6.10.1.5 Test data processing
The calcium salt content is calculated based on the mass fraction w7 of calcium oxide
(CaO), and shall be calculated according to Formula (7):
Where:
V – value of volume of the potassium permanganate standard titration solution
consumed by titration, in mL;
c – accurate value of the concentration of potassium permanganate standard titration
solution, in mol/L;
6.12.2 Reagents or materials
6.12.2.1 Hydrochloric acid.
6.12.2.2 N-butanol.
6.12.2.3 Potassium thiocyanate solution: 30g/L.
6.12.2.4 Iron standard solution: 1mL solution contains 0.1mg of iron (Fe).
Pipette 10mL of iron standard solution prepared according to HG/T 3696.2 into a
100mL volumetric flask; dilute to the mark with water; and shake well. This solution is
prepared before use.
6.12.3 Apparatus
Colorimetric tube: 50mL.
6.12.4 Test procedures
6.12.4.1 Preparation of test solution
Take 5g±0.01g of sample; place it in a 100mL beaker; add about 25mL of water; and
heat the solution on an electric stove. Take off; cool; add 5mL of hydrochloric acid; and
transfer all to a colorimetric tube.
6.12.4.2 Test
Add 10mL of potassium thiocyanate solution and 10mL n-butanol to the test solution;
shake for about 30s; and place when the layer appears; the color of the organic layer
shall be no darker than the standard colorimetric solution.
The standard colorimetric solution is to take 1.00mL of iron standard solution; except
that no sample is added; the other operations and the used reagents are the same as
the test solution.
6.13 Determination of pH
6.13.1 Principle
According to the Nernst equation, the ion activity is proportional to the electrode
potential; so, the relationship curve between the electrode potential and the activity
maybe established for the measured solution; and the hydrogen ion concentration (pH)
may be determined by measuring the potential.
(Red)
m1- value of mass of sieve residue, in g.
The arithmetic mean of the parallel determination results is taken as the determination
result; and the absolute difference between the two parallel determination results shall
be no more than 0.2%.
6.15 Determination of looseness
6.15.1 Principle
Store the bagged samples in the stack for a certain period of time; freely fall from a
certain height on a hard surface; and weigh the mass of the sample left on the sieve
after sieving.
6.15.2 Apparatus
6.15.2.1 Test sieve: It is 950mm long and 600mm wide; and is equipped with a wooden
frame about 120mm high; and the screen aperture is 4.75mm.
6.15.2.2 Stopwatch.
6.15.2.3 Platform scale: 10kg, with a division value of 0.1kg.
6.15.3 Test procedures
From the bagged products in the warehouse where the storage period in stack is no
more than 3 months; select the seventh layer of bagged products from top to bottom
for testing sample.
After weighing the test sample, use a mechanical or manual method to freely drop it
from a height of 1m onto a flat, hard surface. Turn the bag over, then pour the sample
in the bag onto the test sieve; and sieve at a frequency of 1s-1. The sieving stroke is
about 400mm, the sieving time is 1min; and a stopwatch is used to accurately time.
After sieving, wight the mass of the sieve residue. The number of test bags shall be no
less than 3 bags.
6.15.4 Test data processing
The looseness is calculated based on the mass fraction w12 of the sample with a
particle size of less than 4.75mm, and shall be calculated according to Formula (12):
Where:
the entire batch of products shall be unqualified.
7.5 Use the rounding-off value comparison method stipulated in GB/T 8170 to
determine whether the inspection result meets this Standard.
8 Markings and Labels
8.1 The packaging bags of potassium perchlorate for industrial use shall have a firm
and clear mark, the contents of which include manufacturer name, address, product
name, type, grade, net content, batch number or production date, this standard number,
"oxidative substance" mark specified in Clause 3 of GB 190-2009, the "fear of sun"
and "fear of rain" marks specified in Clause 2 of GB/T 191-2008.
8.2 Each batch of potassium perchlorate for industrial use that leaves the factory shall
be accompanied by a quality certificate, the contents of which include name of the
manufacturer, address, product name, type, grade, net content, batch number or
production date, and this Standard number.
8.3 In addition to the quality certificate, the qualified products in each batch or in each
sales unit of Type-II potassium perchlorate for industrial use that leave the factory shall
also be accompanied by a product use reminder, the contents of which include "If this
product is used to manufacture fireworks, firecrackers, the use amount of potassium
perchlorate shall ensure that the chlorate in pyrotechnics complies with the provisions
of 5.6.1.1 in GB 10631-2013” words, as well as the potassium perchlorate contents
and chlorate contents in this batch of products.
9 Packaging, Transportation and Storage
9.1 The packaging type of the potassium perchlorate product for industrial use shall
comply with the provisions of Table 1 in GB 12268-2012; and the limited mass of the
packaging shall comply with the provisions of Appendix A in GB 12463-2009. When
using rail transportation, its packaging shall also comply with the provisions of the
Interim Provisions on the Administration of Transport of Railway Dangerous Goods.
The inner packaging shall adopt polyethylene plastic bag. After the air in the bag is
exhausted, the mouth of the bag is tightly tied. The packaging quality of potassium
perchlorate products for industrial use shall satisfy the Class-II packaging performance
test specified in GB 12463-2009. The net content of each piece is 25 kg or 50 kg. When
users have special requirements for packaging specifications, it can be negotiated
between the supplier and the purchaser. The packaging type shall comply with the
provisions of Table 1 in GB12268-2012; and the limited quality of the packaging shall
comply with the provisions of Appendix A in GB 12463-2009.
9.2 The transportation of potassium perchlorate for industrial use shall comply with the
......
 
(Above excerpt was released on 2020-07-13, modified on 2021-06-07, translated/reviewed by: Wayne Zheng et al.)
Source: https://www.chinesestandard.net/PDF.aspx/HGT3247-2017