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GB/T 534-2014 English PDF (GBT534-2014)

GB/T 534-2014 English PDF (GBT534-2014)

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GB/T 534-2014: Sulphuric acid for industrial use

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.
GB/T 534-2014
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 71.060.30
G 11
Replacing GB/T 534-2002
Sulphuric acid for industrial use
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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: 10??g/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 10??g~100??g. 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: 1??g/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: 0.1??g/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 0??g~0.5??g, or the arsenic content is 0??g~5??g. 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: 2??g/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 4??g), 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: 20??g/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: 1??g/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: 10??g/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 10??g of mercury. Prepare this solution when it is required.
5.8.2.2.8 Mercury standard solution: 1??g/mL or 0.1??g/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 fr...

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