Some standard content:
Chemical Industry Standard of the People's Republic of China
HG/T2692—95
Sulfuric acid for batteries
Published on April 11, 1995
Ministry of Chemical Industry of the People's Republic of China
Implemented on January 1, 1996
W Chemical Industry Standard of the People's Republic of China
Sulfuric acid for batteries
Subject content and scope of application
HG/T2692—95
Replaces GB4554—84
This standard specifies the technical requirements, test methods, inspection rules, marking, packaging, transportation and safety requirements for sulfuric acid for batteries. This standard applies to sulfuric acid for batteries.
Molecular formula: H2SO
Relative molecular mass: 98.08 (according to the international relative atomic mass in 1991) 2 Reference standards
GB190 Dangerous goods packaging mark
GB/T601 Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB/T603 Preparation of preparations and products used in test methods for chemical reagents GB1250 Expression and determination methods of limit values GB/T6682
Specifications and test methods for water used in analytical laboratories GB/T11198.1
GB/T11198.2
GB/T 11198.3
GB/T11198.5
GB/T 11198.6
GB/T 11198.11
GB/T 11198.12
GB/T11198.14
3Product categories
Industrial sulfuric acid
Industrial sulfuric acid
Industrial sulfuric acid
Industrial sulfuric acid
Industrial sulfuric acid
Industrial sulfuric acid
Determination of sulfuric acid content and calculation of free sulfur trioxide content in oleumTitration methodAsh Determination of gravimetric method
O-phenanthroline spectrophotometric method
Determination of iron content
Determination of arsenic content
Triethyldithiocarbamate silver photometric methodDetermination of arsenic content
Gu Cai method
Determination of nitrogen oxides2,4-xylenol spectrophotometric methodDetermination of sulfur dioxide contentIodometric method
Determination of transparency
Sulfuric acid for batteries is divided into concentrated sulfuric acid and dilute sulfuric acid. 4 Technical requirements
Battery sulfuric acid shall meet the requirements specified in Table 1: Approved by the Ministry of Chemical Industry of the People's Republic of China on April 11, 1995 and implemented on January 1, 1996
W.bzsoso.coD Item
Sulfuric acid (HSO) content, %
Ash content, %
Manganese (Mn) content, %
Iron (Fe) content, %
Arsenic (As) content, %
Chlorine (C1) content, %
Nitrogen oxide (as N) content, %
Ammonium (NH) content, %Www.bzxZ.net
Sulfur dioxide (SO2) content, %
Copper (Cu) content, %
Potassium permanganate reducing substances (0) content, %Transparency, mm
5Test method
HG/T2692-95
Dilute sulfuric acid
Superior quality
First-class quality
Superior quality
Concentrated sulfuric acid
The reagents and water used in this standard are analytically pure reagents and meet the requirements of grade 3 water specified in GB/T6682 unless otherwise specified.
5.1 Determination of sulfuric acid content
Test according to the provisions of GB/T11198.1. 5.2 Determination of ash
Test according to the provisions of GB/T11198.2. Chapter 6 "Allowable Difference" is changed to:
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference of the parallel determination results is not more than 0.007% for concentrated sulfuric acid and not more than 0.003% for dilute sulfuric acid. 5.3 Determination of manganese content
5.3.1 Summary of method
After evaporating the sample to dryness, dissolve it with sulfuric acid, phosphoric acid and water, add sodium periodate and heat, use silver ions as catalyst to oxidize manganese into permanganic acid, measure the absorbance of permanganic acid, and calculate the manganese content. 5.3.2 Reagents and solutions
The distilled water used in the preparation of the solution and the entire determination process should be treated in advance. Add a small amount of sulfuric acid to the distilled water to make it acidic, add potassium permanganate solution until it turns purple-red, and distill it once using a distillation device. During the treatment process, be careful not to contact organic matter. 2
W.5.3.2.1 Phosphoric acid (GB/T1282);
HG/T2692—95
5.3.2.2 Sulfuric acid (GB/T625) solution: 1+1; 5.3.2.3 Nitric acid (GB/T626) solution: 1+1; 5.3.2.4 Silver nitrate (GB/T670) solution: 10g/L; 5.3.2.5 Sodium periodate (HG/T3—1157) saturated solution: about 100g/L; 5.3.2.6 Disodium ethylenediaminetetraacetate (EDTA for short) (GB/T1401) solution: 50g/L5.3.2.7 Manganese standard solution: 1mL contains 0.100mg manganese. Weigh 0.100g of metallic manganese into a 200mL beaker, add 10mL of nitric acid solution (5.3.2.3) and 2mL of sulfuric acid solution (5.3.2.2), heat to dissolve, and evaporate to dryness. After cooling, add water to dissolve, transfer to a 1000mL volumetric flask, dilute to scale with water, shake well, and set aside.
5.3.2.8 Manganese standard solution: 1mL contains 0.010mg manganese. Take 50.0mL of manganese standard solution (5.3.2.7), place it in a 500mL volumetric flask, dilute to scale with water, and shake well. Prepare this solution when using.
5.3.3 Instrument
Spectrophotometer.
5.3.4 Analysis steps
5.3.4.1 Drawing of working curve
8. Take 5 50mL beakers, add 2.0, 4.0, 6.0, 8.0, 10.0mL manganese standard solution (5.3.2.8) in turn, and heat and concentrate to about 5mL as needed.
b. After cooling, add 2.5mL sulfuric acid solution (5.3.2.2), 0.3mL phosphoric acid (5.3.2.1), 1mL silver nitrate solution (5.3.2.4) and 7mL sodium periodate solution (5.3.2.5), cover with blood on the surface and boil on the electric stove for 2min; after cooling, transfer to a 25mL volumetric flask, dilute to the scale with water, and shake well. This is solution A. c. Take part of solution A in a 2cm absorption cell, use water as a reference, and measure the absorbance A1 at a wavelength of 530nm. d. Add 2 to 3 drops of EDTA solution (5.3.2.6) to the remaining solution A, shake vigorously to make the purple-red color of permanganate fade. Immediately take part of this liquid and place it in a 2cm absorption cell. Using water as a reference, measure the absorbance A2 at a wavelength of 530nm. Subtract the absorbance A2 from the absorbance A to obtain the absorbance As.
e. Use the mass of manganese as the horizontal coordinate and the corresponding absorbance A: as the vertical coordinate to draw a working curve. 5.3.4.2 Determination
a. Weigh about 100g of sample (accurate to 1g) in a 300mL beaker, heat and evaporate to dryness, cool slightly, add a small amount of water and heat to dissolve, cool, filter in a 50mL beaker, heat and concentrate to 5mL, and then operate according to the procedures of 5.3.4.1b to 5.3.4.1d to measure the absorbance A3.
b. Find the corresponding mass of manganese from the working curve. If the mass of manganese is less than 0.020mg or greater than 0.100mg, change the amount of sample weighed and re-measure.
5.3.5 Expression of analysis results
The manganese (Mn) content X1 expressed as mass percentage is calculated according to formula (1): Xi=mX10×100
Wherein: m—the mass of manganese in the test solution obtained from the working curve, mg; m—the mass of the sample, g.
5.3.6 Permissible difference
The arithmetic mean of the parallel determination results is taken as the determination result. (1)
The absolute difference of the parallel determination results is not greater than 0.000006% for the superior grade of concentrated sulfuric acid and dilute sulfuric acid, and not greater than 0.00005% for the first grade of concentrated sulfuric acid.
5.4 Determination of iron content
The test shall be carried out in accordance with the provisions of GB/T11198.3. The "Allowable Difference" in Chapter 9 is changed to:
HG/T2692-95
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results is not more than 0.0007% for the superior grade of concentrated sulfuric acid and dilute sulfuric acid; and not more than 0.002%.
5.5 Determination of arsenic content Diethyl dithiocarbamate silver photometric method (arbitration method) Inspection is carried out in accordance with the provisions of GB/T11198.5. The "allowable difference" in Chapter 8 is changed to:
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results is not more than 0.000006% for the superior grade of concentrated sulfuric acid and dilute sulfuric acid; the first grade of concentrated sulfuric acid is not more than 0.000.05%.
5.6 Determination of arsenic content Gu Cai method
Inspection is carried out in accordance with the provisions of GB/T11198.6. 5.7 Determination of chlorine content
5.7.1 Summary of the method
The sample is diluted with water, and nitric acid and silver nitrate react with chloride ions to form a silver chloride turbid solution. Compare it with the standard color scale to calculate the chlorine content.
5.7.2 Reagents and solutions
5.7.2.1 Chlorine-free sulfuric acid: Heat sulfuric acid (GB/T625) until white smoke is emitted to drive out the Cl- before use. 5.7.2.2 Nitric acid (GB/T626) solution: 1+2; 5.7.2.3 Silver nitrate (GB/T670) solution: c(AgNOs)=0.1mol/L; Prepare according to GB/T601 and store in a brown bottle.
5.7.2.4 Chlorine standard solution: 1mL contains 0.100mg chlorine; Weigh 0.2103g of potassium chloride (GB/T646 high-grade pure) dried at 500℃ for 1h, dissolve in water, transfer to a 1000mL volumetric flask, dilute to scale with water, shake well, and set aside. 5.7.2.5 Chlorine standard solution: 1mL contains 0.010mg chlorine; dilute with chlorine standard solution (5.7.2.4), prepare the solution when using. 5.7.3 Instrument
Glass colorimetric tube with stopper, volume 50mL.
5.7.4 Analysis steps
Weigh about 5g sample (accurate to 0.1g), add to a beaker containing 25mL water under cooling conditions, and transfer to the colorimetric tube after cooling. Add 1mL nitric acid solution (5.7.2.2), 2mL silver nitrate solution (5.7.2.3), dilute to the scale with water, and shake well. Let stand in the dark for 20min.
According to the above operation, use chlorine-free sulfuric acid (5.7.2.1) instead of the sample to prepare standard color scales, containing 0.020, 0.040, 0.060, and 0.080mg chlorine in turn.
The chlorine content is determined by visual turbidimetry.
5.7.5 Expression of analysis results
The chlorine (C1) content X2 expressed as a mass percentage is calculated according to formula (2): mX10-8
(2)
HG/T2692-95
Wherein: m——the mass of chlorine (CI) in the standard color scale equivalent to the turbidity of the test solution, mg; mo—the mass of the sample, g.
5.8 Determination of nitrogen oxide content
The test is carried out in accordance with the provisions of GB/T11198.11. The "allowable difference" in Chapter 8 is changed to:
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results is not more than 0.00006% for the superior grade of concentrated sulfuric acid, not more than 0.0004% for the first grade; and not more than 0.000006% for the dilute sulfuric acid.
5.9 Determination of ammonium content
5.9.1 Summary of the method
After adding sodium hydroxide to the sample to make it strongly alkaline, steam distill it, take out part of the distillate, add phenol sodium nitrosoferrocyanide and sodium hypochlorite to generate blue indigophenol, and measure its absorbance to calculate the ammonium content. 5.9.2 Reagents and solutions
5.9.2.1 Potassium iodide (GB/T1272);
5.9.2.2 Hydrochloric acid (GB/T622) solution: 1+120;5.9.2.3 Sodium hydroxide (GB/T629) solution: 4g/L5.9.2.4 Ammonia-free sodium hydroxide solution: 300g/L; Prepare according to Article 4.1.4 of GB/T603.
5.9.2.536% acetic acid (HG/T3-1095) solution: 1+1; 5.9.2.6 Starch solution: 10g/L,
5.9.2.7 Phenol sodium nitrosoferricyanide solution; weigh 5g phenol (GB/T339) and 0.025g sodium nitrosoferricyanide (GB/T634) and dissolve them in water, dilute with water to 500mL, store in a cool and dark place, valid within 1 month. 5.9.2.8 Sodium thiosulfate standard titration solution: c (Na2S20s) = 0.05mol/L; prepare and calibrate according to Article 4.6 of GB/T601, and then accurately dilute by 1 time. 5.9.2.9 Sodium hypochlorite (analytical or chemically pure) solution: contains 1 g/L of available chlorine. a. Quantification of available chlorine in sodium hypochlorite
Absorb 10.0 mL of sodium hypochlorite and place it in a 250 mL volumetric flask, dilute to the mark with water, and shake well. Draw 10.0 mL of this solution and place it in a 250 mL conical flask, add water to about 100 mL, add 12 g of potassium iodide (5.9.2.1) and 6 mL of acetic acid solution (5.9.2.5), plug the bottle, shake well, place in a dark place for about 5 min, and titrate with sodium thiosulfate standard titration solution (5.9.2.8) until the solution turns light yellow. Add 3 mL of starch solution (5.9.2.6) as an indicator, and titrate until the blue disappears as the end point. At the same time, perform a blank test under the same operating conditions. The available chlorine content is calculated according to formula (3). A=25×(Vi-V)·oX0. 035×
Wherein: A—effective chlorine content, g/L; V1—volume of sodium thiosulfate standard titration solution consumed in titration, mL; V2—volume of sodium thiosulfate standard titration solution consumed in blank test titration, mL; actual concentration of sodium thiosulfate standard titration solution, mol/L; Vs
—volume of sodium hypochlorite used, mL;
(3)
The mass of effective chlorine equivalent to 1.00mL sodium thiosulfate standard titration solution [c(NazS20s)=1.000mol/L], expressed in grams.
b. Preparation of solution
HG/T2692—95
Weigh 1.5g sodium hydroxide (GB/T629) solid, dissolve it in about 50mL water, add sodium hypochlorite (analytical grade or chemical 100
pure), the volume is (/L)mL of effective chlorine, add water to 100mL, and prepare the solution when it is used. 5.9.2.10 Ammonium (NH) standard solution: 1mL contains 0.100mg ammonium; weigh 0.297g ammonium chloride (GB/T658) (accurate to 0.001g), dissolve it in water, transfer it into a 1000mL volumetric flask, dilute it to the scale with water, shake it well, and set aside.
5.9.2.11 Ammonium (NH) standard solution: 1mL contains 0.002mg ammonium; draw 20.0mL of ammonium standard solution (5.9.2.10), place in a 1000mL volumetric flask, dilute to scale with water, and shake well. Prepare this solution when using.
5.9.2.12 Methyl red-methylene blue mixed indicator solution. Prepare according to Article 4.5.7 of GB/T603.
5.9.3 Apparatus
5.9.3.1 A water vapor distillation apparatus with ground glass connection, as shown in Figure 1, including: a dehydrator;
a distillation flask with a capacity of 500mL, a steam inlet and outlet conduit and a separating funnel with a polytetrafluoroethylene piston, the separating funnel is equipped with a stopper to plug the condenser tube, and a glass tray is provided at the bottom to prevent the condensate outside the tube from flowing into the conical flask d. Conical flask, volume 250mL,
Electric furnace, connected to the voltage-regulating transformer, heating power can be adjusted. Yanqi Import
Figure 1 Ammonium content determination device
5.9.3.2 Spectrophotometer.
5.9.4 Analysis steps
5.9.4.1 Drawing of working curve
Take 6 50mL volumetric flasks, add 0, 3.0, 6.0, 9.0, 12.0, 15.0mL ammonium standard solution (5.9.2.11) in turn, dilute with water to about 25ml, add 5mL phenol nitroso ferrocyanide sodium solution (5.9.2.7), shake well. Add 5mL sodium hypochlorite solution (5.9.2.9b), dilute with water to the scale, shake well, and place at room temperature for 2h. 6
WHG/T2692—95
b. Use a 0.5 cm absorption cell at a wavelength of 640 nm and a blank solution as a reference to measure the absorbance of the solution. c. Use the mass of ammonium as the horizontal axis and the corresponding absorbance as the vertical axis to draw a working curve. 5.9.4.2 Determination
Assemble the instrument as shown in Figure 1.
a. Add 10 mL of hydrochloric acid solution (5.9.2.2) and 40 mL of water to a conical flask (5.9.3.1d), and insert the lower end of the condenser (5.9.3.1c) to the bottom of the solution.
b. Weigh about 50 g of the sample (accurate to 0.1g), slowly add it to the distillation flask (5.9.3.1b) containing 50mL of water. c. Add a few drops of methyl red-methylene blue indicator solution (5.9.2.12) to the distillation flask (5.9.3.1b), slowly add ammonia-free sodium hydroxide solution (5.9.2.4) from the separatory funnel until the solution turns green, and then add 30mL in excess. d. Heat the distillation flask (5.9.3.1b), and after the solution begins to boil, allow steam from the steam generating bottle to pass into the distillation flask (5.9.3.1b) for steam distillation. Control the distillation rate to be about 3-5mL per minute. When the solution in the conical flask (5.9.3.1d) reaches about 180mL, stop distillation.
e. Transfer the solution in the conical flask (5.9.3.1d) into a 250mL volumetric flask, dilute to the mark with water, and shake well. This is solution A. f. Take 25.0 mL of L A solution and place it in a 100 mL beaker, add a few drops of methyl red-methylene blue indicator solution (5.9.2.12), and titrate with sodium hydroxide solution (5.9.2.3) to obtain the milliliters of sodium hydroxide solution (5.9.2.3) required for neutralization. g. Take another 25.0 mL of L A solution and place it in a 50 mL volumetric flask, add the milliliters of sodium hydroxide solution (5.9.2.3) required for neutralization obtained by (5.9.4.2f), neutralize the solution, add 5 mL of sodium nitrosoferricyanide solution (5.9.2.7), and shake well. Follow 5.9.4.1a from "Add 5 mL of sodium hypochlorite solution (5.9.2.9),..." to... and let stand for 2 hours. ” and 5.9.4.1b procedures to measure absorbance A1.
hWhile carrying out the above determination procedures, do not add sample and carry out blank test according to 5.9.4.2a to 5.9.4.2g procedures to measure absorbance A2. Subtract absorbance A2 from absorbance A1 to obtain absorbance A3.i. According to absorbance A, the corresponding ammonium mass can be obtained from the working curve. If absorbance A: exceeds the range of the working curve, appropriately reduce the number of milliliters of solution absorbed by 5.9.4.2g and re-measure according to the following procedures of 5.9.4.2f. 5.9.5 Expression of analysis results
The ammonium (NH) content X expressed as mass percentage is calculated according to formula (4): Xx=250×10-×100
Where: m is from The ammonium mass of the test solution is found on the working curve, mg; mo is the mass of the sample, g.
5.9.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results is not more than 0.0005% for concentrated sulfuric acid and not more than 0.0002% for dilute sulfuric acid. 5.10 Determination of sulfur dioxide content
The test shall be carried out in accordance with the provisions of GB/T11198.12. The "allowable difference" in Chapter 7 is changed to:
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results is not more than 0.0004%. 5.11 Determination of copper content
5.11.1 Summary of the method
(4)
After the sample is evaporated to dryness , dissolve with sulfuric acid, add diammonium hydrogen citrate solution, neutralize with ammonia water, then add diammonium hydrogen citrate solution, complex with copper, measure the absorbance of the complex, and calculate the copper content. 7
W.bzsoso.coI5.11.2 Reagents and solutions
HG/T2692—95
5.11.2.1 Sulfuric acid (GB/T625) solution: 1+1; 5.11.2.2 Ammonia water (GB/T631) solution: 1+15.11.2.3 Diammonium hydrogen citrate (HG/T3—1465) solution: 100g/L, 5.11.2.4 Diammonium hydrogen citrate solution: 1g/L; Weigh 0.5g of diammonium hydrogen citrate, place it in a beaker, and add 50mL95% ethanol (G B/T679) and 50mL warm water, heat in a water bath, and stir until dissolved. If there is insoluble matter, filter, transfer to a 500mL volumetric flask, dilute with water to the mark, and shake well. 5.11.2.5 Nitric acid (GB/T626) solution: 1+1; 5.11.2.6 Copper standard solution: 1mL contains 0.100mg copper; weigh 0.100g of metallic copper (content above 99.9%, accurate to 0.001g), place in a 200mL beaker, add 20mL nitric acid solution (5.11.2.5), and heat to dissolve, then add 20mL sulfuric acid solution (5.11.2.1), slowly heat until white smoke appears to drive out all nitric acid, cool, dissolve in water, transfer to a 1000mL volumetric flask, dilute with water to the mark, shake, and set aside. 5.11.2.7 Copper standard solution: 1mL containing 0.010mg3 of copper is diluted with copper standard solution (5.11.2.6). This solution is prepared when used. 5.11.2.8 Phenolphthalein (GB/T10729) indicator solution: 1g/L. 5.11.3 Instrument
Spectrophotometer.
5.11.4 Analysis steps
5.11.4.1 Drawing of working curve
Take 6 100mL beakers and add 0, 1.0, 2.0, 3.0, 4.0, 5.0mL of copper standard solution (5.11.2.7) in sequence. a.
Heat slowly, evaporate to dryness until no white smoke is emitted, and place to cool: c. Add 5mL of sulfuric acid solution (5.11.2.1), heat to dissolve, cool and transfer to a 50mL volumetric flask, add 5mL of diammonium hydrogen citrate solution ( 5.11.2.3);
Add 2~3 drops of phenolic acid indicator solution (5.11.2.8), add ammonia solution (5.11.2.2) while shaking until it turns slightly red, and then cool to 30~15℃;
Add 10mL of dicyclohexanone oxalyl solution (5.11.2.4), dilute to the scale with water, shake well, and let it stand for about 10min; e.
f. Use a 2cm absorption cell, at a wavelength of 600nm, with water as the reference, to measure the absorbance of the solution; name. Use the copper mass as the horizontal axis and the corresponding absorbance minus the blank solution as the vertical axis to draw a working curve. 5.11.4.2 Determination
a. Weigh about 3g of sample (accurate to 0.01g), transfer to a 100mL beaker, and perform the following operations according to 5.11.4.1b to 5.11.4.1f to measure the absorbance A1.
b. While performing the above determination procedures, do not add sample, perform a blank test according to 5.11.4.1c to 5.11.4.1f, measure the absorbance A2, and subtract the absorbance A2 from the absorbance A to obtain the absorbance As. c. According to the absorbance As, find the corresponding copper mass from the working curve. If the absorbance A: exceeds the range of the working curve, the amount of sample weighed in 5.11.4.2a should be appropriately adjusted, and the determination should be repeated according to 5.11.4.1b to 5.11.4.1f. 5.11.5 Expression of analysis results
The copper (Cu) content X6 expressed as mass percentage is calculated according to formula (5): Xg=mX10-8
Wherein: m——the copper mass of the test solution obtained from the working curve, mg; mo——the mass of the sample, g.
W.bzsoso.coI5.11.6 Allowable difference
HG/T2692-95
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.00006% for the superior grade of concentrated sulfuric acid and dilute sulfuric acid; and not exceed 0.0007% for the first grade of concentrated sulfuric acid.
5.12 Determination of the content of potassium permanganate reducing substances 5.12.1 Method summary
Inject potassium permanganate solution into the sample, add excess ammonium ferrous sulfate solution, and then back-titrate with potassium permanganate solution to determine the content of potassium permanganate reducing substances.
5.12.2 Reagents and solutions
5.12.2.1 Sulfuric acid (GB/T625) solution: 1+17; 5.12.2.2 Ammonium ferrous sulfate (GB/T661) solution: cLNH,Fe(SO,)2J=0.01mol/L. Weigh about 4g of ammonium ferrous sulfate and dissolve it in 1000mL of sulfuric acid solution (5.12.2.1). 5.12.2.3 Potassium permanganate (GB/T643) standard titration solution: c (1/5KMnO) = 0.01 mol/L Prepare, calibrate and dilute according to the provisions of Article 4.12 of GB/T601. 5.12.3 Analysis steps
5.12.3.1 Accurately pipette 5.0 mL of potassium permanganate standard titration solution (5.12.2.3) and place it in a 300 mL beaker containing 100 mL of water.
5.12.3.2 Weigh about 40 g of the sample (accurate to 0.01 g) and slowly add it to the beaker while cooling. Note: If the purple-red color of the solution fades after the sample is added, the potassium permanganate standard titration solution (5.12.2.3) 5.0 mL should be changed to 10.0 mL and the above operation should be repeated.
5.12.3.3. Heat to about 55℃, then cool naturally for about 30 minutes, draw 10.0mL of ammonium ferrous sulfate solution (5.12.2.2), place it in the beaker, and immediately titrate with potassium permanganate standard titration solution (5.12.2.3) until it turns pale purple. 5.12.3.4 While carrying out the above determination procedures, do not add sample and carry out blank test according to procedures 5.12.3.1 and 5.12.3.3. 5.12.4 Expression of analysis results
The oxygen (O) content X equivalent to the substance reducing potassium permanganate, expressed as a mass percentage, is calculated according to formula (6): 0. 008 × (Vi-V,) × 100
Wherein: V1——total volume of potassium permanganate standard titration solution consumed in the determination, mL; V2——total volume of potassium permanganate standard titration solution consumed in the blank test, mL; c——actual concentration of potassium permanganate standard titration solution, mol/L; (6)
0.008——mass of oxygen equivalent to 1.00mL potassium permanganate standard titration solution [c (1/5KMnO,) = 1.000mol/L], expressed in grams.
mo sample mass, g.
5.12.5 Allowable difference
Take the arithmetic mean of the results of parallel determinations as the determination result. The absolute difference of the parallel determination results shall not exceed 0.0004% for concentrated sulfuric acid and 0.00006% for dilute sulfuric acid. 5.13 Determination of transparency
The test shall be carried out in accordance with the provisions of GB/T11198.14. For the product specification of "dilute sulfuric acid", the height of the transparency tube used shall be 400mm. 6 Inspection rules
6.1 The sulfuric acid for batteries shall be inspected by the quality supervision and inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer shall ensure that each batch of products meets the requirements of this standard.
HG/T2692-95
Each batch of products leaving the factory shall be accompanied by a quality certificate. The content shall include the manufacturer's name, address, product name, trademark, grade, net weight, batch number or production date, proof that the product quality meets this standard and the number of this standard. 6.2 The user has the right to inspect and accept the sulfuric acid for batteries received in accordance with the provisions of this standard. 6.3 All technical indicators listed in this standard are type inspection items. Among them, sulfuric acid content, ash content, iron content, sulfur dioxide content, potassium permanganate reduction substance (O) content and transparency are factory inspection items and should be inspected batch by batch. Under normal production conditions, type inspection should be carried out at least once a quarter.
6.4 The samples for inspection shall be randomly sampled by barrel by the quality inspection department. When the total number of units is less than 500 barrels, the number of sampling units can be directly found according to Table 2; if the total number of units is greater than 500 barrels, the number of sampling units shall be determined by 3 times the cube root of the total number of product units 3N (N is the total number of barrels), and if a decimal is encountered, it shall be rounded up to an integer. The total amount of sampling shall not be less than 1000mL.
Total number of barrels
82~101
102~125
125~151
152~181
Number of sampling barrels
Total number of barrels
182~216
217~254
255~296
297~343
344~394
395~450
451512
Number of sampling barrels
6.5 Mix the samples evenly and immediately put them into two clean, dry glass bottles with ground stoppers. The bottles should be labeled with the manufacturer name, product name, batch number, sampling date and sampler’s name. One bottle is used for inspection and the other bottle is used for reserved samples. 6.6 If one of the indicators in the inspection results does not meet the requirements of this standard, samples shall be taken from barrels with twice the number of sampling units of the same batch of products for re-inspection, and the results shall apply to the entire batch of products. Even if one of the indicators in the re-inspection results does not meet the requirements of this standard, the entire batch of sulfuric acid for batteries shall not be accepted.
6.7 When the supply and demand parties have objections to the quality of the product, they shall be handled in accordance with the provisions of the "Product Quality Law of the People's Republic of China". 6.8 Determine whether the inspection results meet the standards according to the rounded value comparison method specified in GB1250. 7 Marking, packaging, transportation
7.1 The packaging container shall be marked with a mark. The content includes the name of the manufacturer, address, product name, trademark, grade, specification, date of manufacture, batch number, and net weight of the product. It should also have the "corrosive product" mark specified in GB190. 7.2 Sulfuric acid for batteries is packed in ceramic jars (jar thickness 10~20mm) or ceramic bottles (bottle thickness 14~16mm); the outer packaging is a wooden box or a half-lattice box, and the jar or bottle is padded with soft materials; the jar or bottle is sealed with acid-resistant materials. 8 Safety requirements
Sulfuric acid for batteries is a strong acid, corrosive and burning. When operating, protective glasses, gloves and protective clothing must be worn. When sulfuric acid and water are mixed, the acid must be poured into the water, and water must never be poured into the acid. Emergency water sources should be available at the work site. 10
W.bzsoso.coD Additional instructions:
HG/T2692—95
This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the sulfur and sulfuric acid standardization technical unit of the Ministry of Chemical Industry. This standard is drafted by the Research Institute of Nanjing Chemical Industry (Group) Corporation. The main drafters of this standard are Guo Peihua, Qi Yumei, Jiang Minhua and Qian Genyou. This standard adopts the former Soviet Union standard rOCT667-73 "Technical conditions for sulfuric acid for batteries". From the date of implementation of this standard, the former national standard of the People's Republic of China GB4554-84 "Sulfuric acid for batteries" will be invalid. 11
4. The samples for inspection shall be randomly sampled by barrels by the personnel of the quality inspection department. When the total number of units is less than 500 barrels, the number of sampling units can be directly found according to Table 2; if the total number of units is greater than 500 barrels, the number of sampling units shall be determined by 3 times the cube root of the total number of product units, 3N (N is the total number of barrels), and any decimals shall be rounded up to integers. The total amount of sampling shall not be less than 1000mL.
Total number of barrels
82~101
102~125
125~151
152~181
Number of sampling barrels
Total number of barrels
182~216
217~254
255~296
297~343
344~394
395~450
451512
Number of sampling barrels
6.5 Mix the samples evenly and immediately put them into two clean, dry glass bottles with ground stoppers. The bottles should be labeled with the manufacturer name, product name, batch number, sampling date and sampler’s name. One bottle is used for inspection and the other bottle is used for reserved samples. 6.6 If one of the indicators in the inspection results does not meet the requirements of this standard, samples shall be taken from barrels with twice the number of sampling units of the same batch of products for re-inspection, and the results shall apply to the entire batch of products. Even if one of the indicators in the re-inspection results does not meet the requirements of this standard, the entire batch of sulfuric acid for batteries shall not be accepted.
6.7 When the supply and demand parties have objections to the quality of the product, they shall be handled in accordance with the provisions of the "Product Quality Law of the People's Republic of China". 6.8 Determine whether the inspection results meet the standards according to the rounded value comparison method specified in GB1250. 7 Marking, packaging, transportation
7.1 The packaging container shall be marked with a mark. The content includes the name of the manufacturer, address, product name, trademark, grade, specification, date of manufacture, batch number, and net weight of the product. It should also have the "corrosive product" mark specified in GB190. 7.2 Sulfuric acid for batteries is packed in ceramic jars (jar thickness 10~20mm) or ceramic bottles (bottle thickness 14~16mm); the outer packaging is a wooden box or a half-lattice box, and the jar or bottle is padded with soft materials; the jar or bottle is sealed with acid-resistant materials. 8 Safety requirements
Sulfuric acid for batteries is a strong acid, corrosive and burning. When operating, protective glasses, gloves and protective clothing must be worn. When sulfuric acid and water are mixed, the acid must be poured into the water, and water must never be poured into the acid. Emergency water sources should be available at the work site. 10
W.bzsoso.coD Additional instructions:
HG/T2692—95
This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the sulfur and sulfuric acid standardization technical unit of the Ministry of Chemical Industry. This standard is drafted by the Research Institute of Nanjing Chemical Industry (Group) Corporation. The main drafters of this standard are Guo Peihua, Qi Yumei, Jiang Minhua and Qian Genyou. This standard adopts the former Soviet Union standard rOCT667-73 "Technical conditions for sulfuric acid for batteries". From the date of implementation of this standard, the former national standard of the People's Republic of China GB4554-84 "Sulfuric acid for batteries" will be invalid. 11
4. The samples for inspection shall be randomly sampled by barrels by the personnel of the quality inspection department. When the total number of units is less than 500 barrels, the number of sampling units can be directly found according to Table 2; if the total number of units is greater than 500 barrels, the number of sampling units shall be determined by 3 times the cube root of the total number of product units, 3N (N is the total number of barrels), and any decimals shall be rounded up to integers. The total amount of sampling shall not be less than 1000mL.
Total number of barrels
82~101
102~125
125~151
152~181
Number of sampling barrels
Total number of barrels
182~216
217~254
255~296
297~343
344~394
395~450
451512
Number of sampling barrels
6.5 Mix the samples evenly and immediately put them into two clean, dry glass bottles with ground stoppers. The bottles should be labeled with the manufacturer name, product name, batch number, sampling date and sampler’s name. One bottle is used for inspection and the other bottle is used for reserved samples. 6.6 If one of the indicators in the inspection results does not meet the requirements of this standard, samples shall be taken from barrels with twice the number of sampling units of the same batch of products for re-inspection, and the results shall apply to the entire batch of products. Even if one of the indicators in the re-inspection results does not meet the requirements of this standard, the entire batch of sulfuric acid for batteries shall not be accepted.
6.7 When the supply and demand parties have objections to the quality of the product, they shall be handled in accordance with the provisions of the "Product Quality Law of the People's Republic of China". 6.8 Determine whether the inspection results meet the standards according to the rounded value comparison method specified in GB1250. 7 Marking, packaging, transportation
7.1 The packaging container shall be marked with a mark. The content includes the name of the manufacturer, address, product name, trademark, grade, specification, date of manufacture, batch number, and net weight of the product. It should also have the "corrosive product" mark specified in GB190. 7.2 Sulfuric acid for batteries is packed in ceramic jars (jar thickness 10~20mm) or ceramic bottles (bottle thickness 14~16mm); the outer packaging is a wooden box or a half-lattice box, and the jar or bottle is padded with soft materials; the jar or bottle is sealed with acid-resistant materials. 8 Safety requirements
Sulfuric acid for batteries is a strong acid, corrosive and burning. When operating, protective glasses, gloves and protective clothing must be worn. When sulfuric acid and water are mixed, the acid must be poured into the water, and water must never be poured into the acid. Emergency water sources should be available at the work site. 10
W.bzsoso.coD Additional instructions:
HG/T2692—95
This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the sulfur and sulfuric acid standardization technical unit of the Ministry of Chemical Industry. This standard is drafted by the Research Institute of Nanjing Chemical Industry (Group) Corporation. The main drafters of this standard are Guo Peihua, Qi Yumei, Jiang Minhua and Qian Genyou. This standard adopts the former Soviet Union standard rOCT667-73 "Technical conditions for sulfuric acid for batteries". From the date of implementation of this standard, the former national standard of the People's Republic of China GB4554-84 "Sulfuric acid for batteries" will be invalid. 11
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