GB/T 534-2014 (GB/T 534-2024 Newer Version) PDF English
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GB/T 534-2014: PDF in English (GBT 534-2014) GB/T 534-2014
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.060.30
G 11
Replacing GB/T 534-2002
Sulphuric acid for industrial use
工业硫酸
ISSUED ON: JULY 08, 2014
IMPLEMENTED ON: DECEMBER 01, 2014
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 ... 5
2 Normative references ... 5
3 Product classification ... 5
4 Requirements ... 6
5 Test methods ... 7
5.1 General ... 7
5.2 Determination of mass fraction of sulphuric acid in concentrated sulphuric acid ... 7
5.3 Determination of free sulfur trioxide mass fraction in oleum ... 8
5.4 Determination of ash mass fraction ... 9
5.5 Determination of iron mass fraction ... 10
5.6 Determination of mass fraction of arsenic ... 14
5.7 Determination of mass fraction of lead ... 19
5.8 Determination of mass fraction of mercury ... 21
5.9 Determination of transparency ... 27
5.10 Determination of chromaticity ... 29
6 Inspection rules ... 29
7 Marks, transport and storage ... 30
8 Safety ... 31
Annex A (informative) Purification of dithizone reagent ... 32
Sulphuric acid for industrial use
WARNING: Some reagents used in this Standard are toxic or corrosive. Some
operations are dangerous. This Standard does not reveal all possible safety issues.
Users shall use it correctly in strict accordance with relevant regulations and are
responsible for taking appropriate safety and health measures.
1 Scope
This Standard specifies the classification, requirements, test methods, inspection rules
and marks, transportation, storage and safety of sulphuric acid for industrial use.
This Standard applies to sulphuric acid for industrial use produced from pyrite, sulfur,
smelting flue gas or other sulfur-containing raw materials.
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 190-2009, Packing symbol of dangerous goods
GB/T 601, Chemical reagent - Preparations of standard volumetric solutions
GB/T 602, Chemical reagent - Preparations of standard solutions for impurity
GB/T 603, Chemical reagent - Preparations of reagent solutions for use in test
methods
GB/T 610, Chemical reagent - General method for the determination of arsenic
GB/T 6680, General rules for sampling liquid 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 and expression and
judgement of limiting values
3 Product classification
Sulphuric acid for industrial use is divided into concentrated sulphuric acid and fuming
Keep away from light.
5.5.1.2.6 Iron (Fe) standard solution: 0.1mg/mL.
5.5.1.2.7 Iron (Fe) standard solution: 10μg/mL.
Measure 10.00mL of iron standard solution (5.5.1.2.6) into a 100mL volumetric flask.
Use water to dilute to the scale. Shake well. Prepare this solution when it is required.
5.5.1.3 Instruments
Spectrophotometer: with 1cm cuvette.
5.5.1.4 Analysis steps
5.5.1.4.1 Drawing of working curve
Take five 50mL volumetric flasks. Add 0mL, 2.50mL, 5.00mL, 7.50mL, 10.00mL of
iron standard solution (5.5.1.2.7) respectively. Do the following for the solution in each
volumetric flask: Add water to about 25mL. Add 2.5mL of hydroxylamine
hydrochloride solution (5.5.1.2.3) and 5mL of acetic acid-sodium acetate buffer
solution (5.5.1.2.4). After 5min, add 5mL of o-phenanthroline hydrochloric acid
solution (5.5.1.2.5). Use water to dilute to the scale. Shake well. Leave it for
15min~30min to develop color.
At the wavelength of 510nm, use a 1cm cuvette. Use the blank solution without iron
standard solution as a reference. Use a spectrophotometer to determine the absorbance
of the above solution.
Take the mass of iron in the above solution (in micrograms) as the abscissa, and the
corresponding absorbance value as the ordinate, to draw the working curve. Or calculate
a linear regression equation based on the obtained absorbance value.
5.5.1.4.2 Determination
Weigh 10g~20g of specimen, accurate to 0.01g. Put in a 50mL beaker. Evaporate to
dryness on a sand bath (or temperature-controlled hotplate). Cool. Add 2mL of
hydrochloric acid solution (5.5.1.2.2) and 25mL of water. Heat to dissolve the salt.
Transfer to a 100mL volumetric flask. Use water to dilute to the scale. Shake well.
Use a pipette to measure a certain volume of the test solution. Place it in a 50mL
volumetric flask. Make the corresponding iron mass between 10μg~100μg. Add water
to dilute to about 25mL. Then follow the steps in "Add 2.5mL of hydroxylamine
hydrochloride solution (5.5.1.2.3) … develop color" in 5.5.1.4.1.
At a wavelength of 510nm, use a 1cm cuvette. Use the blank solution without iron
standard solution as a reference. Use a spectrophotometer to determine the absorbance
of the test solution.
Measure 10.00mL of iron standard solution (5.5.2.3.2) into a 100mL volumetric flask.
Use water to dilute to the scale. Shake well. Prepare this solution when it is required.
5.5.2.4 Instruments
5.5.2.4.1 Dropping bottle: the capacity is about 30mL.
5.5.2.4.2 Atomic absorption spectrophotometer (with iron hollow cathode lamp).
5.5.2.5 Analysis steps
5.5.2.5.1 Drawing of working curve
Take five 50mL volumetric flasks. Add 0mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL of iron
standard solution (5.5.2.3.3) respectively. Add 25mL of nitric acid solution (5.5.2.3.1)
to each. Use water to dilute to the scale. Shake well.
On an atomic absorption spectrophotometer, according to the working conditions of the
instrument, with air-acetylene flame, carry out zero adjustment with blank solution
without adding iron standard solution. Determine the absorbance of the solution at a
wavelength of 248.3nm.
Take the mass of iron in the above solution (in micrograms) as the abscissa, and the
corresponding absorbance value as the ordinate, to draw the working curve. Or calculate
a linear regression equation based on the obtained absorbance value.
5.5.2.5.2 Determination
Use a dropping bottle filled with specimen. Weigh 4g~10g of specimen by subtraction
method, accurate to 0.01g. Put in a 50mL beaker. Evaporate slowly to dryness on a sand
bath (or an adjustable temperature electric stove). Cool. Add 25mL of nitric acid
solution (5.5.2.3.1). Heat to dissolve the residue. Then evaporate to dryness. Cool. Add
25mL of nitric acid solution to dissolve the residue. Transfer to a 50mL volumetric flask.
Use water to dilute to the scale. Shake well.
On the atomic absorption spectrophotometer, according to the working conditions of
the instrument, with air-acetylene flame, carry out zero adjustment with blank solution
without adding iron standard solution. Measure the absorbance of the solution at a
wavelength of 248.3nm. According to the absorbance value of the test solution, find out
from the working curve or calculate the mass of iron in the teste solution according to
the linear regression equation.
5.5.2.6 Calculation of results
The mass fraction w5 of iron (Fe) is calculated according to formula (5):
Weigh 0.5g of potassium hydroxide. Place it in a 150mL beaker. Add about 50mL of
water to make it completely dissolved. Add the weighed 1.5g of potassium borohydride
[w(KBH4) ≥ 95%]. Use water to dilute to 100mL. Shake well. This solution shall be
stored away from light. Prepare it when it is required.
5.6.1.3.4 Thiourea-ascorbic acid solution: 50g/L.
Weigh 5g of thiourea and ascorbic acid, respectively. Use water to slightly dissolve and
dilute to 100mL.
5.6.1.3.5 Arsenic (As) standard solution: 0.1mg/mL.
5.6.1.3.6 Arsenic (As) standard solution: 1μg/mL.
Measure 1.00mL of arsenic standard solution (5.6.1.3.5) into a 100mL volumetric flask.
Use water to dilute to the scale. Shake well. Prepare this solution when it is required.
5.6.1.3.7 Arsenic (As) standard solution: 0.1μg/mL.
Weigh 10.00mL of arsenic standard solution (5.6.1.3.6) into a 100mL volumetric flask.
Add 20mL of thiourea-ascorbic acid solution (5.6.1.3.4) and 5mL of hydrochloric acid
(5.6.1.3.1). Use water to dilute to the scale. Shake well. Prepare this solution when it is
required.
5.6.1.3.8 Argon gas: the purity shall be above 99.99%.
5.6.1.4 Instruments
Atomic fluorescence photometer (with arsenic hollow cathode lamp).
5.6.1.5 Analysis steps
5.6.1.5.1 Drawing of working curve
According to the amount of arsenic in the specimen, choose one of the following two
curves: the arsenic content is 0μg~0.5μg, or the arsenic content is 0μg~5μg.
Take five 50mL volumetric flasks. Add arsenic standard solution (5.6.1.3.6 or 5.6.1.3.7)
respectively according to Table 3. Then add 2.5mL of hydrochloric acid (5.6.1.3.1),
10mL of thiourea-ascorbic acid solution (5.6.1.3.4). Use water to dilute to the scale.
Shake well.
5.6.2.2.4 Arsenic-free metal zinc: particle size is 0.5mm~1mm or 5mm. Those with a
particle size of 5mm shall be treated with (1+1) hydrochloric acid solution before use.
Then use distilled water to clean.
5.6.2.2.5 Mercury bromide test paper.
5.6.2.2.6 Arsenic standard solution: 0.1mg/mL.
5.6.2.2.7 Arsenic standard solution: 2μg/mL.
Measure 2.00mL of arsenic standard solution (5.6.2.2.6) into a 100mL volumetric flask.
Use water to dilute to the scale. Shake well. Prepare this solution when it is required.
5.6.2.2.8 Lead acetate cotton: Use 200g/L lead acetate solution to soak absorbent cotton.
Take out and let dry at room temperature. Keep in an airtight container.
5.6.2.3 Instruments
Arsenic determination instrument: specifications and devices shall comply with the
provisions of GB/T 610.
5.6.2.4 Analysis steps
5.6.2.4.1 Production of standard color spots
Take 7 Erlenmeyer flasks for arsenic determination. Add 0mL, 0.25mL, 0.50mL,
0.75mL, 1.00mL, 1.50mL, 2.00mL of arsenic standard solution (5.6.2.2.7) respectively.
Add 10mL of sulphuric acid solution (5.6.2.2.1) and a certain amount of water. Make
the volume about 50mL. Then add 2mL of potassium iodide solution (5.6.2.2.2) and
2mL of stannous chloride hydrochloric acid solution (5.6.2.2.3) respectively. Shake
well. Let it stand for 15min. Add 5g of arsenic-free metal zinc (5.6.2.2.4). Immediately
connect the instrument as shown in the diagram of the arsenic determination device in
GB/T 610. Allow the reaction to proceed for 45min. Take out the mercuric bromide test
paper. Indicate the corresponding mass of arsenic. Use molten paraffin to impregnate.
Store in a desiccator.
5.6.2.4.2 Determination
Weigh 20g~30g of specimen (the weighing amount can be increased or decreased
according to the arsenic content in the specimen as appropriate; the arsenic content in
each test solution shall not be greater than 4μg), accurate to 0.01g. Put in a 50mL beaker.
Heat slowly on a sand bath (or a thermostatically adjustable hotplate). Evaporate to
about 5mL. After cooling, transfer it to an Erlenmeyer flask filled with an appropriate
amount of water for the determination of arsenic. Add water to make volume about
50mL. Then add 2mL of potassium iodide solution and 2mL of stannous chloride
hydrochloric acid solution. Shake well. Let it stand for 15min. Add 5g of arsenic-free
metal zinc. Immediately connect the instrument as shown in the diagram of the arsenic
determination device in GB/T 610. Allow the reaction to proceed for 45min. Take out
5.8 Determination of mass fraction of mercury
5.8.1 Dithizone spectrophotometry (arbitration method)
5.8.1.1 Principle
Mercury in the test material is oxidized to divalent mercury ions with potassium
permanganate. Use hydroxylamine hydrochloride to reduce the excess oxidant. Add
hydroxylamine hydrochloride and disodium edetate to eliminate the interference of
copper and iron. In the pH range of 0~2, dithizone reacts with mercury ions to form an
orange chelate. After extraction with chloroform solution, measure the absorbance of
the extraction solution at 490nm.
5.8.1.2 Reagents
5.8.1.2.1 Sulphuric acid solution: 490g/L.
5.8.1.2.2 Acetic acid solution: 360g/L. Use anhydrous acetic acid (glacial acetic acid)
of which the density is about 1.05g/mL to prepare.
5.8.1.2.3 Disodium edetate solution: 7.45g/L.
5.8.1.2.4 Potassium permanganate solution: 40g/L.
5.8.1.2.5 Hydroxylamine hydrochloride solution: 100g/L.
5.8.1.2.6 Dithizone chloroform solution: 150mg/L.
Use chloroform to prepare the solution. Store in an airtight, dry brown bottle. Store in
a dark place below 25°C. It is valid for two weeks.
NOTE: See Annex A for the purification of dithizone reagent.
5.8.1.2.7 Dithizone chloroform solution: 3mg/L.
Measure 5.00mL of dithizone chloroform solution (5.8.1.2.6) into a dry 250mL
volumetric flask. Use chloroform to dilute to the scale. Shake well. Prepare this solution
when it is required. Store in dark, cool place.
5.8.1.2.8 Mercury standard solution: 1mg/mL.
Weigh 1.354g of mercuric chloride. Dissolve in 25mL of hydrochloric acid. Then
transfer to a 1000mL volumetric flask. Use water to dilute to the scale. Shake well.
Keep the solution in a cool place. It is valid for two months.
5.8.1.2.9 Mercury standard solution: 20μg/mL.
Measure 5.00mL of mercury standard solution (5.8.1.2.8). Place it in a 250mL
volumetric flask. Add 5mL of hydrochloric acid. Use water to dilute to the scale. Shake
well. Prepare this solution when it is required.
5.8.1.2.10 Mercury standard solution: 1μg/mL.
Measure 5.00mL of mercury standard solution (5.8.1.2.9). Place it in a 100mL
volumetric flask. Add 2.5mL of hydrochloric acid. Use water to dilute to the scale.
Shake well. Prepare this solution when it is required.
5.8.1.3 Instruments
5.8.1.3.1 Routine instruments for testing: All instruments that have not been used for
mercury content determination, including glass bottles containing reagents and
specimens, shall be washed in the following sequence before use:
a) If there is oil on the wall, scrub it with soap and a brush;
b) Soak in (1+1) nitric acid solution for more than 12hor soak in (1+3) nitric acid
solution for more than 24h. Rinse well with tap water;
c) Use potassium permanganate lotion prepared by mixing 4 sulphuric acid solutions
with a volume concentration of 100g/L and 1 volume of potassium permanganate
solution (5.8.1.2.4) to wash. After repeated rinsing with tap water, rinse with
distilled water.
5.8.1.3.2 Spectrophotometer: with a 3cm cuvette.
5.8.1.4 Analysis steps
5.8.1.4.1 Drawing of working curve
Take six 500mL separatory funnels. Use cotton or filter paper to dry its neck. Tuck in a
small ball of absorbent cotton. Add 0mL, 2.00mL, 4.00mL, 6.00mL, 8.00mL of
mercury standard solution (5.8.1.2.10) into the funnel, respectively. Then treat the
solution in each separatory funnel as follows: Add 20mL of sulphuric acid solution
(5.8.1.2.1). Use water to dilute to about 200mL. Add 1mL of hydroxylamine
hydrochloride solution (5.8.1.2.5), 10mL of acetic acid solution (5.8.1.2.2), 10mL of
disodium edetate solution (5.8.1.2.3) and 20.0mL of dithizone chloroform solution
(5.8.1.2.7). Shake vigorously for 1min. Let it stand for 10min to separate the two phases.
Let out part of the organic phase. Place in a 3cm cuvette. At 490nm wavelength of the
spectrophotometer, use the blank solution without mercury standard solution as a
reference to measure the absorbance of the solution.
Take the mass of mercury in the above solution (in micrograms) as the abscissa and the
corresponding absorbance value as the ordinate, to draw a working curve. Or calculate
a linear regression equation based on the obtained absorbance value.
wavelength of 253.7nm with an atomic absorption spectrophotometer or an ultraviolet
absorption mercury analyzer.
5.8.2.2 Reagents
5.8.2.2.1 Sulphuric acid solution: 490g/L.
5.8.2.2.2 Potassium permanganate solution: 40g/L.
5.8.2.2.3 Hydroxylamine hydrochloride solution: 100g/L.
5.8.2.2.4 Stannous chloride hydrochloric acid solution: 100g/L.
Weigh 25g of stannous chloride. Dissolve in 50mL of hot hydrochloric acid. Transfer
to a 250mL volumetric flask after cooling. Use water to dilute to the scale.
5.8.2.2.5 Iodine solution: 2.5g/L.
5.8.2.2.6 Mercury standard solution: 1mg/mL. The preparation method is the same as
5.8.1.2.8.
5.8.2.2.7 Mercury standard solution: 10μg/mL.
Measure 5.00mL of mercury standard solution (5.8.2.2.6). Place it in a 500mL
volumetric flask. Add 5mL of hydrochloric acid. Use water to dilute to the scale. Shake
well. 1mL of this solution contains 10μg of mercury. Prepare this solution when it is
required.
5.8.2.2.8 Mercury standard solution: 1μg/mL or 0.1μg/mL. According to the amount of
mercury in the specimen, decide which concentration of mercury standard solution to
use. Prepare this solution when it is required.
Use a pipette to pipette a certain amount of mercury standard solution (5.8.2.2.7). Use
(1+105) hydrochloric acid solution to accurately dilute to the corresponding volume.
Shake well.
5.8.2.3 Instruments
5.8.2.3.1 Routine instruments for testing: same as 5.8.1.3.1.
5.8.2.3.2 Dropping bottle: capacity is about 30mL.
5.8.2.3.3 Atomic absorption spectrophotometer or ultraviolet absorption mercury
detector: with low pressure mercury lamp or hollow cathode lamp.
5.8.2.3.4 Blowing (or suction) determination system device: as shown in Figure 1.
5.10 Determination of chromaticity
5.10.1 Reagents
5.10.1.1 Ammonia.
5.10.1.2 Sodium sulfide solution: 20g/L.
5.10.1.3 Gelatin solution: 10g/L.
5.10.1.4 Lead standard solution: 0.1mg/mL.
Weigh 0.1831g of lead acetate. Use water to dissolve. Transfer to 1000mL volumetric
flask. If cloudy, add few drops of acetic acid. Then use water to dilute to the scale.
5.10.2 Analysis steps
5.10.2.1 Preparation of standard chromaticity
Add 10mL of water, 3mL of gelatin solution (5.10.1.3), 2~3 drops of ammonia water
(5.10.1.1), 3mL of sodium sulfide solution (5.10.1.2), and 2.0mL of lead standard
solution (5.10. 1.4) into 50mL colorimetric tube. Then use water to dilute to 20mL.
Shake well.
5.10.2.2 Determination
Add 20mL of specimen to another 50mL colorimetric tube. Visually compare the
chromaticity of the specimen and standard solution colorimetric tubes. If the color of
the specimen is not deeper than the standard color, it shall be qualified.
6 Inspection rules
6.1 Sulphuric acid for industrial use shall be inspected batch by batch by the quality
supervision and inspection department of the manufacturer. The manufacturer shall
ensure that each batch of manufactured products meets the requirements of this
Standard. Each batch of exit-factory products shall be accompanied by a quality
certificate or a product certificate, indicating manufacture’s name, address, product
name, product grade, production date or batch number, reference to this Standard, and
so on.
6.2 For sulphuric acid for industrial use produced from smelting flue gas as raw material,
all items listed in this Standard are exit-factory inspection items.
For sulphuric acid for industrial use produced from other raw materials, all items listed
in this Standard are type inspection items. Among them, the mass fraction of sulphuric
acid or free sulfur trioxide, the mass fraction of ash, the mass fraction of iron,
transparency and chroma are the exit-factory inspection items. Under normal
production conditions, at least one type inspection shall be carried out every quarter.
The mass fractions of arsenic, lead and mercury in the inspection items can be inspected
by a qualified inspection agency.
6.3 Products are inspected by batch. Take each storage tank or daily output as a batch.
Sampling is according to the provisions of GB/T 6680. The total amount of sampling
shall not be less than 500mL. After mixing the obtained specimens evenly, immediately
put them into two clean, dry glass bottles with ground stoppers. Label shall be affixed
on the bottle, indicating the name of the manufacturer, product name, grade, batch
number, sampling date, and the name of the sampler. One bottle is used for inspection.
The other shall be kept for no less than 15 days for reference.
6.4 The inspection results shall be judged whether they conform to this Standard
according to the rounding value comparison method stipulated in GB/T 8170. If one of
the indicators in the inspection results does not meet the requirements of this Standard,
twice the number of samples shall be taken from the storage tank for reinspection. Even
if one of the indicators does not meet the requirements of this Standard in the
reinspection results, the entire batch of products shall be rejected.
6.5 The user has the right to check and accept the received sulphuric acid for industrial
use in accordance with the provisions of this Standard. Verify whether its quality meets
the requirements of this Standard. When the supplier and the purchaser disagree on the
product quality, it shall be inspected by a qualified third-party inspection agency.
7 Marks, transport and storage
7.1 The packaging container of each batch of sulphuric acid leaving the factory shall
have a clear "corrosive substance" mark in accordance with the provisions of GB 190-
2009.
7.2 Sulphuric acid for industrial use shall be transported in special tank trucks (ships).
Tank trucks (ships) shall be cleaned regularly. Sulphuric acid for industrial use can also
be transported in other acid-resistant packaging containers (such as plastic barrels). The
container size depends on the need. Containers shall be sealed with lids of acid-resistant
material.
7.3 Sulphuric acid for industrial use shall be stored separately from flammable and
combustible substances, reducing agents, alkalis, metal powders. Mixed storage is not
allowed.
...... Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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