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GB/T 42391-2023 English PDF (GBT42391-2023)

GB/T 42391-2023 English PDF (GBT42391-2023)

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GB/T 42391-2023: Electrolyte for lead acid storage battery

This document specifies the requirements, determination methods, inspection rules, marking, packaging, transportation, storage and safety requirements of the electrolyte (including colloidal electrolyte) for lead acid storage battery. This document is applicable to the electrolyte (including colloidal electrolyte) for lead acid storage battery. This document does not apply to the electrolyte in lead acid storage battery after disassembly.
GB/T 42391-2023
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 29.220.20
CCS K 84
Electrolyte for Lead Acid Storage Battery
(IEC 62877-1:2016, Electrolyte and Water for Vented Lead Acid Accumulators - Part 1: Requirements for Electrolyte, MOD)
ISSUED ON: MARCH 17, 2023
IMPLEMENTED ON: OCTOBER 1, 2023
Issued by: State Administration for Market Regulation;
Standardization Administration of the PEOPLE Republic of China.
Table of Contents
Foreword ... 3
1 Scope ... 6
2 Normative References ... 6
3 Terms and Definitions ... 7
4 Requirements ... 7
5 Determination Method ... 8
6 Inspection Rules ... 21
7 Marking, Packaging, Transportation and Storage ... 22
8 Safety Requirements ... 22
Appendix A (informative) Comparison of Concentration and Density of Sulfuric Acid ... 23
Electrolyte for Lead Acid Storage Battery
1 Scope
This document specifies the requirements, determination methods, inspection rules, marking, packaging, transportation, storage and safety requirements of the electrolyte (including colloidal electrolyte) for lead acid storage battery.
This document is applicable to the electrolyte (including colloidal electrolyte) for lead acid storage battery.
This document does not apply to the electrolyte in lead acid storage battery after disassembly. 2 Normative References
The contents of the following documents constitute indispensable clauses of this document through the normative references in the text. In terms of references with a specified date, only versions with a specified date are applicable to this document. In terms of references without a specified date, the latest version (including all the modifications) is applicable to this document. GB 190 Packing Symbol of Dangerous Goods
GB/T 622 Chemical Reagent - Hydrochloric Acid (GB/T 622-2006, ISO 6353-2:1983, NEQ) GB/T 625 Chemical Reagent - Sulfuric Acid (GB/T 625-2007, ISO 6353-2:1983, NEQ) GB/T 626 Chemical Reagent - Nitric Acid (GB/T 626-2006, ISO 6353-2:1983, NEQ) GB/T 629 Chemical Reagent - Sodium Hydroxide
GB/T 643 Chemical Reagent - Potassium Permanganate (GB/T 643-2008, ISO 6353-2:1983, NEQ)
GB/T 661 Chemical Reagent - Ammonium Iron (II) Sulfate Hexahydrate (GB/T 661-2011, ISO 6353-3:1987, NEQ)
GB/T 670 Chemical Reagent - Silver Nitrate (GB/T 670-2007, ISO 6353-2:1983, NEQ) GB 1253 Working Chemical - Sodium Chloride
GB 1254 Working Chemical - Sodium Oxalate
GB 1257 Working Chemical - Potassium Hydrogen Phthalate
GB 12595 Working Chemical - Silver Nitrate
In a brightly lit room, conduct a visual inspection on whether the surface of the sample is colorless and transparent.
5.2.2 Density
5.2.2.1 Instrument
Density meter: with a division value of ??? 0.001 g/cm3.
5.2.2.2 Determination steps
Take 250 mL of the specimen in 5.1.2.1, stir it well, then, transfer it into a 250 mL measuring cylinder; put it in a water bath at 25 ???C, let it stand for 20 min. Gently put the density meter into the specimen, wait until it stops sinking, visually observe the tangent line of the concave surface of the liquid, and read the value on the density meter.
The test result shall retain three decimal places.
5.2.3 Determination of sulfuric acid content
5.2.3.1 Principle
Weigh-take or absorb a certain amount of specimen, and use methyl red-methylene blue as a mixed indicator. The end point of titration is pH = 5.4, and the solution turns from purple red to gray green, and the color variation is sensitive and easy to judge.
5.2.3.2 Reagents and solutions
The reagents and solutions required for the test are as follows:
---Methyl red-methylene blue mixed indicator: one portion of 0.2% methyl red ethanol solution is mixed with one portion of 0.1% methylene blue ethanol;
---Potassium hydrogen phthalate (GB 1257): benchmark reagent;
---Phenolphthalein: analytically pure, 0.1% ethanol solution;
---Sodium hydroxide (GB/T 629): analytically pure, standard solution of C (NaOH) = 0.5 mol/L.
a) Preparation: prepare a saturated solution of sodium hydroxide and store it in a plastic bottle, seal it and place it, until the solution becomes clear. Take 26 mL of the supernatant and place it in 1,000 mL of carbon dioxide-free water, and mix it well; b) Calibration: weigh-take 3 g (accurate to 0.0001 g) of benchmark potassium hydrogen phthalate dried at 105 ???C ~ 110 ???C for 2 h, put it in a 250 mL conical flask, add 80 mL of water and heat it to boiling. Dropwise add 2 drops ~ 3 drops of 0.1% phenolphthalein indicator, and use sodium hydroxide solution of C (NaOH) = 0.5 mol/L to titrate it, until the solution turns pink, which is the end point. 5.2.4 Determination of reduced potassium permanganate (calculated by O) content 5.2.4.1 Principle
Inject excess potassium permanganate solution into the specimen to thoroughly oxidize the reducing substance; use ferrous ammonium sulfate solution to perform back titration, so as to obtain the content of reduced potassium permanganate.
5.2.4.2 Reagents and solutions
The reagents and solutions required for the test are as follows:
---Sulfuric acid (GB/T 625): analytically pure, 1 + 1 solution and solution with a density of 1.200 g/cm3;
NOTE: see Appendix A for the comparison of the concentration and density of sulfuric acid. ---Sodium oxalate (GB 1254): benchmark reagent;
---Ferrous ammonium sulfate solution (GB/T 661): analytically pure, C [(NH4)2Fe(SO4)2] = 0.01 mol/L. Weigh-take 4 g of (NH4)2Fe(SO4)2 ??? 6 H2O and dissolve in 100 mL of 1 + 1 sulfuric acid solution, and use water to dilute to 1,000 mL;
---Potassium permanganate standard solution (GB/T 643): analytically pure, C (1/5 KMnO4) = 0.1 mol/L. This standard solution is used to prepare a standard solution of C (1/5 KMnO4) = 0.01 mol/L.
a) Preparation: weigh-take 3.30 g of potassium permanganate, dissolve it in 1,050 mL of water, slowly boil it for 20 min ~ 30 min and place it in the dark for a week. Use glass wool to filter it, and store the filtrate in a brown bottle with a ground stopper. b) Calibration: weigh-take 0.2 g of benchmark sodium oxalate dried at 105 ???C ~ 110 ???C for 2 h, accurate to 0.0001 g, and dissolve it in 50 mL of pure water. Add 8 mL of concentrated sulfuric acid, use potassium permanganate standard solution of C (1/5 KMnO4) = 0.1 mol/L to titrate it, and when it approaches the end point, heat to 70 ???C ~ 80 ???C, continue titration, until the solution turns pink and maintains for 30 s, meanwhile, carry out a blank test.
c) Calculation: the concentration of 0.1 mol/L potassium permanganate solution of C (1/5 KMnO4) shall be calculated in accordance with Formula (3).
Where,
m---the mass of the weighed sodium oxalate, expressed in (g);
V---the volume of potassium permanganate solution used, expressed in (mL); M (1/2 Na2C2O4)---the mass of 0.5 mol of sodium oxalate, expressed in (g/mol). d) Preparation of 0.01 mol/L potassium permanganate standard solution: use pure water to accurately dilute the prepared potassium permanganate standard solution of C (1/5 KMnO4) = 0.1 mol/L to C (1/5 KMnO4) = 0.01 mol/L.
5.2.4.3 Instruments
Commonly used laboratory instruments: 250 mL conical flask and burette, etc. 5.2.4.4 Determination steps
5.2.4.4.1 Correction of ratio
The ratio of the volume (mL) of potassium permanganate standard solution of C (1/5 KMnO4) = 0.01 mol/L to the volume (mL) of ferrous ammonium sulfate solution of C [(NH4)2Fe(SO4)2] = 0.01 mol/L, expressed in K, shall be corrected by the following method and calculated in accordance with Formula (4).
Weigh-take 40 g (accurate to 0.001 g) of diluted sulfuric acid with a density of 1.200 g/cm3 (the average value of the electrolyte density, so that the reaction is carried out at the same acidity), place it in a 250 mL conical flask. Use a burette to accurately add 10 mL of potassium permanganate standard solution of C (1/5 KMnO4) = 0.01 mol/L, and use 0.01 mol/L ferrous ammonium sulfate solution to perform the titration.
Where,
V---the volume of potassium permanganate standard solution used, expressed in (mL); V1---the volume of ferrous ammonium sulfate solution used, expressed in (mL). 5.2.4.4.2 Determination of specimen
Weigh-take 40 g (accurate to 0.001 g) of the specimen in 5.1.2.1, place it in a 250 mL conical flask; use a burette to accurately add 10 mL of potassium permanganate standard solution of C (1/5 KMnO4) = 0.01 mol/L and heat to 70 ???C ~ 80 ???C. Stop heating, and cool to room temperature, (when the specimen appears discolored, re-sampling shall be considered, and the quantity of specimens to be weighed shall be reduced) accurately add 10 mL of ferrous ammonium sulfate solution of C [(NH4)2Fe(SO4)2] = 0.01 mol/L. Immediately use potassium permanganate standard solution of C (1/5 KMnO4) = 0.01 mol/L to titrate it, until it turns light purple red, which is the end point.
5.2.4.5 Result calculation
solution contains 0.5 mg of chlorine; Solution B: 1 mL of standard solution contains 0.05 mg of chlorine.
Solution A: accurately weigh-take 0.8245 g of benchmark sodium chloride burned at 500 ???C ~ 600 ???C for 1 h, dissolve it in 50 mL of water, then, transfer it into a 1,000 mL volumetric flask; use water to wash it and dilute to the scale, then, shake it well. Solution B: accurately draw 10 mL of Solution A and put it in a 100 mL volumetric flask; use water to dilute to the scale, and shake it well.
5.2.5.3 Instruments
Commonly used laboratory instruments: 50 mL colorimetric tube, 100 mL volumetric flask and 1,000 mL volumetric flask, etc.
5.2.5.4 Determination steps
5.2.5.4.1 Preparation of standard color gradation
Successively add 0.0 mL, 0.4 mL, 0.8 mL, 1.2 mL, 1.6 mL and 2.0 mL of chlorine standard solution B to six 50 mL colorimetric tubes, then, use a pipette to add 30 mL of chlorine-free diluted sulfuric acid with the same density as the specimen. Then, respectively add 2 mL of 1 + 4 nitric acid and 2 mL of 2% silver nitrate, and shake it well. Place it in the dark for 20 min. 5.2.5.4.2 Determination of specimen
Weigh-take 30 g of specimen in a 50 mL colorimetric tube, accurate to 0.001 g (m); add 2 mL of 1 + 4 nitric acid and 2 mL of 2% silver nitrate. Compare it with the standard color gradation, and adopt the method of visual turbidimetry to determine the chlorine content. 5.2.5.5 Result calculation
The chlorine content, which is expressed in mass fraction X3 and mg/L, shall be calculated in accordance with Formula (6):
Where,
m1---the chlorine content of the chlorine standard solution with the same turbidity as the specimen, expressed in (mg);
m---the mass of the specimen, expressed in (g);
??---the density of the specimen, expressed in (g/cm3).
The calculation result shall retain three decimal places.
5.2.6 Determination of iron, copper, manganese, nickel, antimony, bismuth, cadmium, cobalt, zinc and chromium content
5.2.6.1 Instrument
Atomic absorption spectrophotometer.
5.2.6.2 Preparation of standard solution
The preparation of standard solution is shown in Table 3.
5.2.6.3 Specimen preparation
Use an elongated pipette to take 20 mL of the sample in 5.1.2.1 in a 250 mL volumetric flask, dilute it to the scale, and take the blank solution as a reference. On the atomic absorption spectrophotometer, use the acetylene-air flame, and in accordance with the wavelengths in Table 3, successively determine the concentration of the blank C0 and the specimen C1. 5.2.6.4 Result calculation
The iron, copper, manganese, nickel, antimony, bismuth, cadmium, cobalt, zinc and chromium content shall be calculated in accordance with Formula (7):
Where,
C x---the concentration of a certain element specimen, expressed in (mg/L); C1---the read concentration in the determination of a certain element, expressed in (???g/mL); C0---the blank concentration in the determination of a certain element, expressed in (???g/mL); n---the dilution ratio of the specimen (take 12.5).
5.2.7 Determination of titanium, mercury, tin and selenium content
5.2.7.1 Instrument
Inductively coupled plasma emission spectrometer (ICP).
5.2.7.2 Preparation of standard solution
See the preparation of standard solution in Table 3.
5.2.7.3 Specimen preparation
Use an elongated pipette to take 20 mL of the sample in 5.1.2.1 in a 250 mL volumetric flask, dilute it to the scale, and take the blank solution as a reference. On the inductively coupled plasma emission spectrometer, successively determine the concentration of the blank C0 and 5.3 Determination Method for Colloids
5.3.1 Appearance
In a brightly lit room, conduct a visual inspection on whether the color of the appearance of the specimen is uniform.
5.3.2 pH
Take a piece of pH test paper universal, dip it into the specimen, after 1 s, take it out, compare it with the standard color plate and read the pH.
The test result shall retain an integer.
5.3.3 Density
5.3.3.1 Instrument
Density meter: 1.000 g/cm3 ~ 2.000 g/cm3, with a division value of 0.005 g/cm3. 5.3.3.2 Determination steps
Take 250 mL of the specimen in 5.1.2.2, thoroughly stir it, then, transfer it into a 250 mL graduated cylinder. Place the graduated cylinder in a water bath at 25 ???C ??? 1 ???C and maintain the temperature constant; let it stand for 20 min, so that the air bubbles can overflow. Gently put the density meter into the test solution, wait for it to stop sinking, then, visually observe the tangent line of the concave surface of the specimen solution, and read the value on the density meter.
The test result shall retain three decimal places.
5.3.4 Determination of silicon dioxide content
5.3.4.1 Instrument
High-temperature chamber electric resistance furnace, with the temperature controlled at 950 ???C ~ 1,000 ???C.
5.3.4.2 Reagent and solution
Hydrochloric acid (GB/T 622): analytically pure, with a density of 1.190 g/cm3. 5.3.4.3 Determination steps
Weigh-take 10 g of specimen (accurate to 0.0001 g) in a 120 mL porcelain, slowly add 10 mL of concentrated hydrochloric acid with a density of 1.190 g/cm3. Place the solution on a water bath at 80 ???C, heat and concentrate it to dryness, steam it for 1 h, then, remove and cool it. Add 5 mL of concentrated hydrochloric acid, heat it to slight boiling, then, add 20 mL of hot water, and immediately use a medium-speed quantitative filter paper to filter it into a 250 mL volumetric flask (the filtrate can be used for the determination of impurities, for example, iron). Use hot water to wash the precipitate and the filter paper, until there is no chloride ion (use silver nitrate to test it); use water to dilute it to the scale and shake it well. Place the precipitate and the filter paper in a porcelain crucible with a constant mass and carefully incinerate it. In the high-temperature chamber electric resistance furnace at 950 ???C ~ 1,000 ???C, burn it for 30 min, then, place it in a desiccator to cool to room temperature, until reaching a constant mass (otherwise, the burning shall be performed again). 5.3.4.4 Result calculation
The content of silicon dioxide, which is expressed in mass fraction X4, shall be calculated in accordance with Formula (9):
Where,
G1---the dry weight of the precipitate of silicon dioxide, expressed in (g); G---the weight of the specimen, expressed in (g).
The calculation result shall retain an integer.
5.3.5 Determination of iron content
See 5.2.6.
NOTE: when being transferred to a 250 mL volumetric flask, the colloidal specimens need to be filtered.
5.3.6 Determination of chlorine content
5.3.6.1 Instruments and equipment
The instruments and equipment required for the test are as follows:
---High-temperature chamber electric resistance furnace, with the temperature controlled at 500 ???C ~ 600 ???C;
---Constant-temperature drying oven.
5.3.6.2 Reagents and solutions
The reagents and solutions required for the test are as follows:
---Potassium chromate (HB/T 3440): analytically pure, 5% solution. Weigh-take 5 g (accurate to 0.1 g) of potassium chromate, and dissolve it in a small amount of water; (the instrument needs to be calibrated before use).
6 Inspection Rules
6.1 To prepare the electrolyte for lead acid storage batteries, the concentrated sulfuric acid used shall comply with the requirements of HG/T 2692.
6.2 The water used to prepare the electrolyte for lead acid storage batteries shall comply with the requirements of GB/T 42323-2023.
6.3 The electrolyte for lead acid storage batteries shall be inspected by the manufacturer?€?s quality department in accordance with the stipulations of this document, and the manufacturer shall ensure that each batch of products complies with the requirements of this document. 6.4 Each batch of products exiting the factory shall be accompanied by a quality certificate, including the manufacturer?€?s name, address, product name, trademark, grade, net weight, batch No. or production date, as well as a certificate proving that the product quality complies with this document and the serial No. of this document.
6.5 All technical indicators listed in this document are type inspection items. Among them, the four items of the electrolyte (appearance, sulfuric acid content, iron content and reduced potassium permanganate content) and the four items of the colloid (masterbatch) (appearance, pH, silicon dioxide content and iron content) are exit-factory inspection items, which shall be inspected batch by batch. Under the circumstance of normal product, at least one type inspection shall be carried out every quarter.
6.6 The samples used for inspection shall be sampled in barrels. When the obtained specimens are evenly mixed, immediately put them into two clean and dry glass bottles with a ground stopper. Labels shall be affixed on the bottles, indicating the manufacturer?€?s name, product name, batch No., date of sampling and name of sampler. One bottle is used for inspection and the other bottle is reserved.
6.7 The batch rules of the electrolyte for lead acid storage batteries shall be: acceptance inspection by batches and calculation by liters. The volume of each batch is 400 L ~ 8,000 L. Sample selection shall be carried out in accordance with 5.1.2 or determined through negotiation between both sides.
6.8 The judgment rule for the electrolyte for lead acid storage batteries is that if one of the indicators in the inspection results does not comply with the requirements of this document, then, double the sampling size from the same batch of products and repeat the inspection of all performances; the results are applicable to the entire batch of products. If one of the indicators in the re-inspection results does not comply with the requirements of this document, then, the entire batch of products shall be determined as disqualified.
7 Marking, Packaging, Transportation and Storage
7.1 Marking
The product packaging container shall be marked with the manufacturer?€?s name, address, product name, trademark, grade, specification, date, batch No. and product net weight. In addition, there shall be a ?€?CORROSIVES?€? mark as specified in GB 190.
7.2 Packaging
The products can be packed in acid-resistant plastic barrels for transportation. The size of the container depends on the manufacturer?€?s demands, and the container must be sealed with an acid-resistant cover.
7.3 Transportation
During transportation, the products must not be heavily pressed, turned upside down or bumped, and avoid exposure to the sun. During loading and unloading...

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