HG/T 3811-2006 English PDF (HG/T3811-2006)

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HG/T 3811-2006: Methods of test for bromide for industrial use
HG/T 3811-2006
HG
CHEMICAL INDUSTRY STANDARD
OF THE PEOPLE'S REPUBLIC OF CHINA
ICS 71.060.50
G 04
File No.. 18156-2006
Methods of test for bromide for industrial use
ISSUED ON. JULY 26, 2006
IMPLEMENTED ON. MARCH 1, 2007
Issued by. National Development and Reform Commission
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Test methods ... 4 
Annex A (Informative) Determination method for electric potential
titration end-point and data record example ... 16 
Foreword
Please note that some contents in this standard may involve patents. The issuer of this
standard does not undertake the responsibility to identify these patents.
Annex A of this standard is informative.
This standard was proposed by China Petroleum and Chemical Industry Federation.
This standard shall be under the jurisdiction of National Standardization Technical
Committee of Chemical (SAC/TC63/SC1).
The main drafting organizations of this standard. Qingdao Entry-exit Inspection and
Quarantine Bureau, Jiangsu World Chemical Co., Ltd., Shandong Weifang Longwei
Industrial Co., Ltd., Tianjin Chemical Research and Design Institute.
The main drafters of this standard. ZHAO Zuliang, XU Shanquan, YANG Wenhua, MOU
Lanting, LI Guangming.
Methods of test for bromide for industrial use
1 Scope
This standard specifies the test method of bromide for industrial use.
This standard is applicable to bromide for industrial use. This standard specifies the
determination technology of product. When preparing the test solution, the standards
related to the analyzed product shall be referenced to conduct the necessary revision to
this standard, so as to make it more appropriate for the determination of product.
2 Normative references
The articles contained in the following documents have become part of this standard when
they are quoted herein. For the dated documents so quoted, all subsequent modifications
(including all corrections) or revisions made thereafter do not apply to this standard.
However, the parties who reach an agreement according to this standard are encouraged
to study whether the latest versions of these documents may be used. For the undated
documents so quoted, the latest versions (including all modification sheets) apply to this
document.
GB/T 3049-1986 Chemical products for industrial use - General method for determination
of iron content - 1,10-Phenanthroline spectrophotometric method [ISO 6685.1982(E) IDT]
GB/T 6682-1992 Water for analytical laboratory use - Specification and test methods (eqv
ISO 3696.1987)
GB/T 9724-1988 Chemical reagent - General rules for the determination of pH
HG/T 3696.1 Inorganic chemical products - Preparations of standard volumetric solutions
for chemical analysis
HG/T 3696.2 Inorganic chemical products - Preparations of standard solutions for
chemical analysis
HG/T 3696.3 Inorganic chemical products - Preparations of reagent solutions for chemical
analysis
3 Test methods
3.1 Safety warning
Some reagents used in this test are poisonous or corrosive. Special attention must be
paid during operation! If splashed to skin, wash with plenty of water. If the condition is
severe, take the injured to hospital for professional medical treatment.
3.2 General stipulations
Unless otherwise specified, all the reagents used in this standard refer to analytic
reagents; water is Grade-3 water as stipulated in GB/T 6682. Unless otherwise specified,
all the standard titration solutions, standard impurity solutions, preparations and products
used in the test shall be in accordance with HG/T 3696.1, HG/T 3696.2 or HG/T 3696.3
for preparation.
3.3 Determination of bromide content
3.3.1 Potentiometric titration (arbitration)
3.3.1.1 Method summary
Under the nitric acid condition, add the starch indicator; use 216-type silver electrode as
the indicating electrode, 217-type double salt bridge saturated calomel electrode as the
reference electrode; use the standard silver nitrate solution for titration.
3.3.1.2 Reagent
3.3.1.2.1 Nitric acid solution. 1+4.
3.3.1.2.2 Standard silver nitrate titration solution. c(AgNO3), about 0.1 mol/L.
3.3.1.2.3 Starch solution. 10g/L (prepared before use).
3.3.1.3 Instruments
3.3.1.3.1 216-type silver electrode.
3.3.1.3.2 217-type double salt bridge saturated calomel electrode.
3.3.1.4 Analytical procedure
Take 0.4g of sample, accurate to 0.01g, into a 250ml beaker. Add 100ml of water for
dissolution; add 10ml of nitric acid and 10ml of starch indicator solution. Use 216-type
silver electrode as the indicating electrode; use 217-type double salt bridge saturated
calomel electrode as the reference electrode. The standard silver nitrate titration solution
is used for titration. At the early stage of titration, add a certain amount of standard silver
nitrate titration solution. When approaching the end-point, gradually add 0.1ml per time
(increased if necessary). Record the total volume and the corresponding potential E after
each addition of silver nitrate. Calculate the difference Δ2E between the continuously
increased potentials, Δ1E and Δ1E. The maximum value of Δ1E is the titration end-point;
after the end-point, continue to record an additional potential value E.
The data record format and the calculation of the volume of the consumed standard
titration solution (V) when reaching the titration end-point are shown in annex A.
3.3.1.5 Result calculation
Bromide content is counted by the mass fraction w1, its value is expressed by %,
calculated in accordance with formula (1).
m — the mass of specimen, unit. g;
M — the molar mass of bromide, unit. g/mol;
K — the coefficient to convert chloride to bromide;
ω2 — the mass fraction of chloride, unit. %.
3.4 Determination of chloride content
3.4.1 Warning. When determining chloride, sample pre-treatment requires bromine
evaporation. This product is toxic, it must be carried out in the well-ventilated fume
cupboard.
3.4.2 Potentiometric titration (arbitration method)
3.4.2.1 Method summary
Use nitric acid to oxidize bromide ion to bromine; and heat it for evaporation. Under the
nitric acid condition, add the starch indicator; use 216-type silver electrode as the
indicating electrode; use 217-type double salt bridge saturated calomel electrode as the
reference electrode. Use standard silver nitrate titration solution for titration.
3.4.2.2 Reagent
3.4.2.2.1 Nitric acid solution. 2 + 3.
3.4.2.2.2 Starch solution. 10g/L (prepared before use).
3.4.2.2.3 Standard silver nitrate titration solution. c(AgNO3), about 0.05 mol/L or 0.02
mol/L.
3.4.2.3 Instruments
3.4.2.3.1 216-type silver electrode (silver electrode vulcanized);
3.4.2.3.2 217-type double salt bridge saturated calomel electrode.
3.4.2.4 Analytical procedure
Take about 4g of sample, accurate to 0.01g, into in a 250ml beaker. Add 50ml of nitric
acid solution; put it in the water bath (80°C) in the fume cupboard. Heat the beaker until
the yellow color fades away. Use a small amount of water to wash the beaker wall;
continue to heat the beaker for 15min; wait for cooling down; then, add water to 50ml in
the beaker. Add 10ml of starch indicator solution; use 216-type silver electrode as the
indicating electrode and 217-type double salt bridge saturated calomel electrode as the
reference electrode; use standard silver nitrate titration solution for titration. At the early
stage of titration, add a certain am...