Some standard content:
JB/T 10052--1999
This standard is a revision of ZBK84003-89 "Electrolyte for Lead-acid Batteries". The format and rules of this standard are GB/T1.1-1993 to ensure the uniformity of standard writing and its applicability and international exchange. Compared with ZBK84003-89, this standard has the following changes: -Added preface;
-Chapter, section and clause are rearranged according to the changes in content; -4.1 (added sampling);
-4.2 (added appearance inspection).
This standard will replace ZBK84003-89 from the date of implementation. Appendix A of this standard is the appendix of the standard.
This standard is under the jurisdiction of the National Lead-acid Battery Standardization Technical Committee. This standard is drafted by Shenyang Battery Research Institute. The main drafter of this standard: Zhuang Yajing.
This standard was first issued in March 1989 and revised for the first time in 1998. 95
1 Scope
Mechanical Industry Standard of the People's Republic of China
Electrolyte for lead acid storage batteries
Electrolyte for lead acid storage batteriesJB/T 10052-1999
Replaces ZBK84003-89
This standard specifies the requirements, test methods, inspection rules and storage and safety of electrolyte for lead acid storage batteries. This standard applies to electrolyte for lead acid storage batteries. This standard does not apply to electrolyte for sealed lead acid storage batteries. 2 Referenced standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. At the time of publication of the standard, the versions shown are valid. All standards will be revised, and parties using this standard should explore the possibility of using the latest version of the following standards. GB/T 1.4—1988
GB/T 622—1989
GB/T 625—1989
GB/T 626—1989
GB/T 631—1989
GB/T 638—1988|| tt||GB/T 643 — 1988 ||tt | 670—1986
GB 1254—1990
GB/T 1272—1988
GB/T 1294—1993
GB/T 1401—1985||t t||GB/T 2304—1988
GB/T 6685—1986
GB/T 10729-—1989
GB 12595-1990
HG 3--1098—1977
HG 3—1465--1982
Guidelines for standardization work Provisions for the preparation of standards for chemical analysis methods Main chemical reagents
Chemical reagents
Chemical reagents
Chemical reagents
Chemical reagents
Chemical reagents
Chemical reagents
Chemical reagents
Chemical reagents
Chemical reagents
Chemical reagents
Chemical reagents
Chemical reagents
Chemical reagents
Chemical reagents
Chemical reagents
Sodium hydroxide
Stannic chloride
Potassium permanganate
Potassium nitrate
Ammonium persulfate
Ammonium ferrous sulfate
Chloroform
Sodium acetate
Silver nitrate
Working standard reagent (capacity)
Sodium oxalate
Working standard reagent (capacity)
Potassium hydrogen phthalate
Chemical reagent
Chemical reagent
Chemical reagent
Chemical reagent
Chemical reagent
Chemical reagent
Chemical reagent
Potassium iodide
1,10-phenanthroline
Tartaric acid
Disodium ethylenediaminetetraacetic acid| |tt||Arsenic-free zinc
Hydroxyamine hydrochloride
Working standard reagent (capacity)
Chemical reagent
Chemical reagent
Approved by the State Machinery Industry Bureau on 1999-08-0696
Silver nitrate
Acetic acid (36%)
Diammonium hydrogen citrate
Implementation on 2000-01-01
HG 2603-1994
Chemical reagent
HG/T 2692--1995
JB/T 10052-1999
Lead acetate
JB/T10053-1999 Water for lead-acid batteries 3 Requirements
The electrolyte for lead-acid batteries shall meet the requirements of Table 1. Table 1
Content of sulfuric acid (H2SO4)
Density p50℃, g/cm2
Content of ignition residue≤
Content of manganese (Mn)≤
Content of iron (Fe)≤
Content of arsenic (As)≤
Content of chlorine (CI)≤
Content of nitrate (as N)≤
Content of potash (Cu)≤
Reduced permanganate
Content of potassium permanganate
Determination method
4.1 Sampling
4.1.1 Sampling conditions
Name
Content as ○≤
Content as KMnO≤
The samples must be placed in the production site, use site or warehouse at room temperature. 4.1.2 Sampling method
Colorless, transparent
180~480
For the test conducted according to this standard, at least 5I representative electrolyte samples should be taken, and the samples should be filled in a clean, sealed plastic container. 4.1.3 Sample preservation method
The sample must be placed at room temperature, without direct sunlight, and covered to prevent impurities from entering. 4.2 Appearance inspection
4.2.1 Inspection method
Visually inspect the color of the sample surface in a brightly lit room to see if it is colorless and transparent. 4.3 Sulfuric acid content
4.3.1 Principle
Weigh or absorb a certain amount of sample, use methyl red and methylene blue as mixed indicators, the end point is pH 5.4, the solution changes from purple-red to gray-green, and the color change is sensitive and easy to judge.
4.3.2 Reagents and solutions
Methyl red-methylene blue mixed indicator: one part of 0.2% methyl red ethanol solution and one part of 0.1% methylene blue ethanol solution; Potassium hydrogen phthalate (GB1257): standard reagent; 97
JB/T 10052—1999
Phenolic acid (HGB.3039), analytical grade: 0.1% ethanol solution; Sodium hydroxide (GB/T629), analytical grade: standard solution of C(NaOH)=0.5mol/I. a) Preparation: Prepare a saturated solution of sodium hydroxide and store it in a plastic bottle. Seal it and place it until the solution is clear. Take out 26ml of the supernatant and mix it in 1000ml of water without carbon dioxide. b) Calibration: Weigh 3g of standard potassium hydrogen phthalate dried at 105-110℃ for 2h, add 80mL of water to a 250ml conical flask and heat to boiling. Add 2-3 drops of 0.1% phenolic acid indicator and use a hydrogen peroxide with C(NaOH)=0.5mol/I. Titrate the sodium hydroxide solution until the solution turns pink;
c) Calculation: The concentration of sodium hydroxide C(NaOH) is calculated according to formula (1): C(NaOH)
M(KHC.H,O4)
Wherein: m——the mass of potassium hydrogen phthalate weighed, g; V-the amount of sodium hydroxide solution used, mL;
M(KHC.H,O)——the molar mass of potassium hydrogen phthalate, g/mol. 4.3.3 Instruments
——a constant temperature drying oven;
——an electro-optical analytical balance (one ten-thousandth);——a general laboratory instrument.
4.3.4 Determination steps
Accurately aspirate 2mL of the sample (or weigh 2.5g, about 2ml, with a dry small weighing bottle, and wash it with 250ml of water.conical flask), dilute to 80mL with water in a 250mL conical flask, add 2-3 drops of methyl red-methyl blue mixed indicator, and titrate with C (NaOH)-0.5mol/L sodium hydroxide standard solution until the solution changes from purple-red to gray-green. 4.3.5 Calculation of results
The sulfuric acid content Xi is expressed as mass percentage or X2 is expressed as g/L, and is calculated according to formula (2) and (3): C(NaOH)×V× M(1/2 H,SO,)
M(1/2 H2SO/)
C(NaOH) XV X
Wherein: C(NaOH)—concentration of sodium hydroxide standard solution, mol/L; V
—amount of sodium hydroxide standard solution, mL; M(1/2 H,SO)-
—molar mass of sulfuric acid, g/mol;
—mass of sample, g;
V,--volume of sample, mL.
4.4 Ignition residue
4.4.1 Principle
The sample is evaporated and smoked, and then burned at 800℃ for 20min and weighed after cooling. 4.4.2 Instruments
Quartz blood (or magnetic evaporation blood), capacity 100mL; a high temperature furnace, temperature controllable at 800±50℃, a general laboratory instrument.
4.4.3 Determination steps
Burning quartz blood (or magnetic evaporation III) in a high temperature furnace at 800±50℃ for 20min, taking out and cooling slightly, placing in a desiccator to cool to room temperature, weighing, accurate to 0.0001g.
JB/T10052—1999
Use a pipette to draw 50mL of uniform sample, put it in a weighing quartz dish, carefully heat and evaporate until smoke appears, move it into a high temperature furnace, burning at 800±50℃ for 20min, taking out and cooling slightly, placing in a desiccator, cooling to room temperature (about 20-30min), weighing, accurate to 0.0001g.
4.4.4 Calculation of results
The ignition residue content (X) is expressed in g/1 and is calculated according to formula (4): m,-m.
Wherein: ml—mass of residue and quartz blood, g; m.mass of quartz dish, g;
Vi——volume of sample, mL.
4.5 Potassium permanganate reduction substance
4.5.1 Principle
Inject an excess of potassium permanganate solution into the sample to fully oxidize the reducing substance, and back-titrate with ammonium ferrous sulfate solution to calculate the content of potassium permanganate reduction substance.
4.5.2 Reagents and solutions
Sulfuric acid (GB/T625): analytical grade, 1+1 solution and solution with density 1.20 g/cm; Sodium oxalate (GB1254): reference reagent; Ammonium ferrous sulfate (GB/T 661): analytical grade, C［(NH4),Fe（SO)2］=0.01 mol/L solution, weigh 4g (NH), Fe(SO)2·6H2O and dissolve it in 100mL 1+1 sulfuric acid solution, dilute with water to 1000mL; Potassium permanganate (GB/T643): analytical grade, C (1/5KMnO) = 0.1mol/L. Standard solution: (This standard solution is used to prepare the standard solution of C (1/5KMnO4) = 0.01mol/L. a) Preparation
Weigh 3.3g potassium permanganate, dissolve it in 1050ml water, boil gently for 20-30min, place in a dark place for one week, filter with glass wool, and store the filtrate in a brown bottle with a ground-mouth stopper. b) Calibration
Weigh 0.2 g of standard sodium oxalate dried at 105-110℃ for 2 h, accurate to 0.0001 g, dissolve in 50 ml of water, add 8 ml of concentrated sulfuric acid, and titrate with potassium permanganate solution with C (1/5KMnO,) = 0.1 mol/I. When it is close to the endpoint, heat to 70-80℃ and continue titrating until the solution turns pink and maintains it for 30 seconds. At the same time, do a blank test. c) Calculate
The concentration of potassium permanganate C(1/5KMnO4) is calculated according to formula (5): C(1/5 KMnO,)=
Wherein: m is the mass of sodium oxalate weighed, g; V is the amount of potassium permanganate solution used, mL; m
V×M(1/2 Na,C,0.)
M(1/2Na2C2O）--—the molar mass of sodium oxalate, g/mol(5)
When using, dilute the prepared potassium permanganate standard solution with C(1/5KMnO.)=0.1mol/L with water accurately to C(1/5KMnO）=0. 01 mol/L.
4.5.3 Instruments
——General laboratory instruments.
4.5.4 Determination steps
4.5.4.1 Correction of ratio
The ratio of the amount of potassium permanganate standard solution (mL) of C(1/5KMnO)=0.1mol/L to the amount of ammonium ferrous sulfate solution (mL) of C[(NH4),Fe(SO4)=0.01mol/1, expressed as K, is corrected and calculated as follows:99
JB/T 10052—1999
Measure 100ml of dilute sulfuric acid with a density of 1.20, put it in a 250ml conical flask, and accurately add 10ml of potassium permanganate standard solution of C(1/5KMnO4)=0.01mol/L with a burette, and proceed as follows. V
Wherein: V——the amount of potassium permanganate standard solution, mL; Vi——the amount of ammonium ferrous sulfate solution, mL.
4.5.4.2 Sample determination
（6）
Pipette 100mL of sample and put it into a 250mL conical flask. Use a burette to accurately add 10mL of potassium permanganate standard solution (C(1/5KMnO.)=0.01mol/L). Heat to 70~80℃. Cool to room temperature and accurately add 10mL of ammonium ferrous sulfate solution (C[(NH)2Fe（SO4)2］0.01mol/L). Immediately titrate with potassium permanganate standard solution (C(1/5KMnO)=0.01mol/L) until a pale purple color is the end point. 4.5.5 Calculation of results
The content of potassium permanganate reducing substance (X, X) is expressed as gram per liter (g/L) of equimolar oxygen amount n(1/2Oz) or potassium permanganate amount n(1/5KMnO), respectively, and is calculated according to formula (7) and (8): X,-.00xC(1.KMn.)x(V-KV1000...100X 0. 01
Xx0. 0016xC(1/5KMpO)x(V-KV2×1000 *no.+..
Wherein: V—amount of potassium permanganate standard solution, mL; Vi——amount of ammonium ferrous sulfate solution, mL; .. (7)
..·.. (8)
K---1 mL C[(NH4),Fe(SO4)2J=0.01 mol/L of ammonium ferrous sulfate solution is equivalent to C(1/5 KMnO4)-the number of milliliters of potassium permanganate standard solution of 0.01mol/L; C(1/5KMnO4)-the concentration of potassium permanganate standard solution, mol/L; 0.00008-the mass of oxygen (O) equivalent to 1mL C(1/5KMnO4)=0.01mol/l, standard solution, g; 0.000316-the mass of potassium permanganate (KMnO) equivalent to 1mL C(1/5KMnO4)=0.01mol/L standard solution, g. 4.6 Nitrate (including nitrite) content 4.6.1 Principle
In sulfuric acid solution, strychnine and nitrate produce yellow compounds, and their color intensity is basically proportional to the nitrate concentration. The biggest advantage of this method is that it is simple and fast. It is not interfered by chloride ions and nitrites. However, strong oxidants and reducing agents may interfere. In addition, there are many factors that affect the determination results, mainly the temperature of the solution. degree, followed by air temperature, sulfuric acid concentration, beaker size, speed of pouring reagents, placement time and light effects, etc. Standard colorimetry and sample must be carried out simultaneously, and the analytical conditions and steps must be as consistent as possible, so that the measured results are accurate.
4.6.2 Reagents and solutions
Hydrochloric acid (GB/T622): analytical grade;
-sulfuric acid (GB/T625): analytical grade, density 1.20g/cm2, use a measuring cup to measure 500ml of concentrated sulfuric acid, slowly add it to a beaker containing 75mL of water, and stir continuously with a glass rod, cool to room temperature, and cover the sulfuric acid solution tightly for storage; strychnine para-nitrobenzenesulfonic acid reagent, 1g strychnine sulfate [(C23H26N.O4)2H2SO4·7H,O] or 0.78g strychnine C23H2sNzO4 and 0.1g para-aminobenzenesulfonic acid [CH(NH2)(SO3H)],Dissolve in 70mL hot water, add 3mL concentrated hydrochloric acid, cool and dilute to 100mL, this solution can be used for several months; Potassium nitrate (GB/T 647): analytical grade, solution A: 1 ml. Nitrogen (N) 0.1mg, solution B: 1mL standard solution containing nitrogen (N) 0.01mg.
Solution A: weigh 0.7218g KNO3 in a 300mL beaker, dissolve in sulfuric acid solution with a density of 1.20g/cm2, transfer to a 1000mL volumetric flask, dilute to the scale, and shake well. Solution B: When using, accurately aspirate 10mL of solution A, put it in a 100ml volumetric flask, dilute to the scale with dilute sulfuric acid with a density of 1.20g/cm2, and shake well.
4.6.3 Instruments
Spectrophotometer;
General laboratory instruments.
4.6.4 Determination steps
4.6.4.1 Drawing of standard curve
JB/T 10052-1999
Into six 25mL colorimetric tubes, add 0.0, 0.4, 0.8, 1.2, 1.6, 2.0mL of potassium nitrate standard solution B in sequence, dilute to 2mL with dilute sulfuric acid with a density of 1.20g/cm2, add 1mL of strychnine p-aminobenzenesulfonic acid reagent and 10mL of sulfuric acid solution to each tube, then carefully invert back and forth 6 times to mix, and place in a dark place for 10±1min. At this time, add 10mL of water to each tube, invert back and forth 6 times as above, and place the mixture in a dark place for 20-30min.
Put part of the solution in 1cm colorimetric blood, take the reagent blank solution as reference, measure the absorbance of each solution in turn at a wavelength of 510nm, use nitrogen (N) to represent the nitrate (NO2) content as the horizontal coordinate, and the corresponding absorbance as the vertical coordinate to draw a standard curve. 4.6.4.2 Determination of sample
Pick 2mL of sample, put it in a 25mL colorimetric tube, add a few drops of potassium permanganate solution with C (1/5KMnO) = 0.01mol/L until it turns slightly red and keep for 3min.
Note: If only nitrate is measured, potassium permanganate oxidation can be omitted. Add 1mL of strychnine p-aminobenzenesulfonic acid reagent, and operate simultaneously according to the method of drawing a standard curve. The measured absorbance is compared with the standard curve to obtain the corresponding nitrate nitrogen content.
4.6.5 Calculation of results
The nitrate content (X) is expressed as g/L of nitrogen (N) and is calculated according to formula (9): X=
2X1000
Wherein: m—the amount of nitrate nitrogen obtained from the sample absorbance curve, mg. 4.7 Chloride content
4.7.1 Principle
·(9)
In a slightly acidic nitric acid solution, chloride ions react with silver ions to form a turbid microprecipitate of silver chloride colloid, which is uniformly suspended in the solution. The chlorine content is determined by turbidimetry. This method can measure chlorine content as low as 0.1ug per milliliter. 4.7.2 Reagents and solutions
Sulfuric acid (GB/T625): analytical grade, density 1.20g/cm3, chlorine-containing solution. Prepared with sulfuric acid heated to emit white sulfur trioxide smoke and drive out all chloride ions;
Nitric acid (GB/T626): analytical grade, 1+4 solution; -Silver nitrate (GB/T670): analytical grade, 2% solution; Sodium chloride, liquid A: 1mL. Contains 0.5mg chlorine (Cl), liquid B: 1mL standard solution containing 0.05mg chlorine. Liquid A: Accurately weigh 0.8245g of standard sodium chloride burned at 500~~600℃ for 1h, dissolve in 50mL water and transfer to a 1000ml volumetric flask, wash with water and dilute to the scale, shake well. Liquid B: Accurately draw 10ml of liquid A, put it in a 100mL volumetric flask, dilute to the scale with water, shake well. 4.7.3 Instruments
- General laboratory instruments.
4.7.4 Determination steps
4.7.4.1 Preparation of standard color scale
Add 0.0, 0.4, 0.8, 1.2, 1.6, 2.0 ml of chlorine standard solution B to six 50 ml colorimetric tubes, dilute to 50 ml with chlorine-free dilute sulfuric acid of the same density as the sample, add 2 ml of 1+4 nitric acid and 2 ml of 2% silver nitrate, shake well. Let stand in the dark for 20 min.
4.7.4.2 Determination of sample
JB/T10052—1999
Pull 50 ml of the sample into a 50 ml colorimetric tube, add 2 ml of 1+4 nitric acid, and carry out the following operations simultaneously as for the preparation of standard color scale, and determine the chlorine content by visual turbidimetry.
4.7.5 Calculation of results
Chlorine content (X) is expressed in g/L and is calculated according to formula (10): mi
X=vxi00×1000
Wherein: m!
Chlorine content of the same turbidity standard solution as the sample, mg; Vi-sample volume, ml.
4.8 Iron content
4.8.1 Principle
Directly absorb the sample and neutralize it with ammonium hydroxide, and use hydroxylamine hydrochloride to reduce high-valent iron and eliminate the interference of copper at the same time. In a solution with a pH of 3~~5, low-valent iron reacts with o-phenanthroline to form an orange-red complex, which is used to determine iron by colorimetry. There are few impurities in the solution and it is not interfered with by the analysis. 4.8.2 Reagents and solutions
Hydroxylamine hydrochloride (HG3-967): analytical grade, 10% solution - Ammonium hydroxide (GB/T631): analytical grade, 1+1 solution; Sodium acetate (GB/T694) - Acetic acid (GB/T676) buffer: analytical grade, pH 4, weigh 20g NaAC·3H,O and dissolve it in appropriate amount of water, add 134mL 36% HAC, dilute with water to 500mL, and mix well; - O-phenanthroline (GB/T1293): analytical grade, 0.1% solution, weigh 0.1g o-phenanthroline in a small amount of water, add two drops of 1+1 hydrochloric acid, dissolve it and dilute with water to 100ml, and store it in a brown bottle; Iron standard solution, solution A, 1ml contains 0.1mg iron, solution B 1ml contains 0.01mg iron. Liquid A: Weigh 0.1000g of pure iron wire with an iron content of more than 99.99% into a 100ml beaker, add 10ml of 1+1 nitric acid and dissolve it with slight heat, wash the beaker wall with a small amount of water, heat to remove nitrogen oxides, transfer to a 1000ml volumetric flask after cooling, wash with C (HNO:) = 1mol/I. nitric acid, dilute to the scale, and shake to hook.
Liquid B: When using, accurately draw 10ml of Liquid A, put it in a 100mL volumetric flask, dilute to the scale with water, and shake well. 4.8.3 Instruments
- General laboratory instruments.
4.8.4 Determination steps
4.8.4.1 Drawing of standard curve
In seven 50mL volumetric flasks, add 0.0, 1.0, 2.0, 3.0, 4.0, 5.0, 6.0mL of iron standard solution B in turn, dilute with water to 35mL, 2mL of 10% hydroxylamine hydrochloride solution, adjust the solution to pH 4~5 with 1+1 ammonium hydroxide solution, add 5mL of sodium acetate acetate buffer, 5mL of 0.1% o-phenanthroline solution, place at room temperature for 30min (or heat in a boiling water bath for 2~3min, cool), dilute with water to the scale, and shake well.
Take part of the solution in 1cm colorimetric blood, use the reagent blank solution as reference, measure the absorbance of each solution in turn at a wavelength of 510nm, and draw a standard curve with the iron content (in mg) as the horizontal coordinate and the corresponding absorbance as the vertical coordinate. 4.8.4.2 Determination of samplebzxz.net
Pipette 1-2 ml of sample, dilute to 30 ml with water in a 50 ml volumetric flask, add 2 ml of 10% hydroxylamine hydrochloride solution, and perform the following operations according to the method of drawing a standard curve. Take the reagent blank solution as the reference, and obtain the corresponding iron content from the absorbance measured on the standard curve. Perform a reagent blank test at the same time according to the above method.
4.8.5 Calculation of results
The iron content (X) is expressed in g/L and is calculated according to formula (11): m
X=V,X1000×
Where: mi
The iron content obtained by the sample absorbance on the standard curve, mg; .. (11)
V, — sample volume, mL.
4.9 Manganese content
4.9.1 Principle
JB/T 10052--1999
In a hot solution of mixed acid, silver nitrate is used as a catalyst and ammonium persulfate is used to oxidize low-valent manganese to heptavalent purple permanganate (MnO), and the absorbance is measured at a wavelength of 530nm. EDTA is added to the oxidized test solution to fade the color of the heptavalent manganese, which is used as a colorimetric reference solution to eliminate the influence of the color of the sample base solution.
4.9.2 Reagents and solutions
—Mixed acid: Add 50 mL of analytical grade sulfuric acid (GB/T625) to 500 mL of water. After cooling, add 50 nL of analytical grade phosphoric acid (GB/T1282) and 50 mL of analytical grade nitric acid (GB/T626). At room temperature, add 1 g of analytical grade silver nitrate (GB/T670), dilute with water to 1000 mL, and dissolve and mix well.
Ammonium persulfate (GB/T655): analytical grade, 15% solution; Disodium ethylenediaminetetraacetic acid (GB/T1401), analytical grade, 5% solution; Manganese standard solution, Solution A: 1 mL contains 0.1 mg manganese, Solution B: 1 mL contains 0.01 mg manganese. Liquid A: Accurately weigh 0.1000g of manganese metal treated with 1+1 hydrochloric acid and anhydrous ethanol, with a content of more than 99.99%, and add 5mL of 1+1 nitric acid to a 100ml beaker. After dissolving with slight heat, wash the wall of the beaker with water until it boils slightly to remove nitrogen oxides. After cooling, transfer it to a 1000mL volumetric flask, wash it with water and dilute it to the scale, and shake it well. Liquid B: Accurately pipette 10mL of Liquid A into a 100mL volumetric flask, dilute it to the scale with water, and shake it well. 4.9.3 Instruments
—Constant temperature water bath;
—General laboratory instruments.
4.9.4 Determination steps
4.9.4.1 Drawing of standard curve
Add 0.0, 1.0, 2.0, 3.0, 4.0, 5.0 mL of manganese standard solution B to six 50 mL volumetric flasks, dilute each to 20 mL with water, add 20 mL of mixed acid, 8 mL of 15% ammonium persulfate solution, and mix well. Place in a boiling water bath, heat for 1 min under boiling, remove and place for 1 min, cool to room temperature in tap water, dilute to scale with water, and shake. Take part of the solution in a 3 cm colorimetric dish, and use the remaining color developing solution that has been added with 1 to 2 drops of 5% EDTA to fade the color of heptavalent manganese as a reference. Measure the absorbance of each solution at a wavelength of 530 nm, and draw a standard curve with the manganese content (in mg) as the horizontal coordinate and the corresponding absorbance minus the blank as the vertical coordinate. 4.9.4.2 Determination of sample
Pipette 50mL or 100mL of sample (depending on the manganese content) into a 250ml beaker, heat and evaporate until white smoke is emitted and dry. Cool slightly, add 20ml of mixed acid, heat and slightly boil to dissolve for 2min, cool slightly, transfer the solution into (if turbid or precipitated, filter with slow filter paper) a 50ml volumetric flask, wash the beaker with water, control the volume to 40mL, add 8mL of 15% ammonium sulfate solution, and mix well. The following operation is carried out according to the method of drawing a standard curve, subtract the measured absorbance from the reagent blank absorbance, and check the corresponding manganese content on the standard curve. Perform a reagent blank test at the same time according to the above method. 4.9.5 Calculation of results
Manganese content (X) is expressed in g/L and is calculated according to formula (12): X = V1000 × 1000
Wherein; ml is the amount of manganese obtained from the sample absorbance curve, mg; Vi is the sample volume, mL.
4.10 Copper content
4.10.1 Principle
JB/T10052-1999
In an ammonia medium with a pH of 8 to 9.8, using diammonium hydrogen citrate and tartaric acid as masking agents, divalent copper is complexed with dicyclohexanone oxalyl dihydrazone solution (abbreviated as BCO) to form a blue complex with a maximum absorption at 580600nm. Common elements in the sample do not interfere with the determination. 4.10.2 Reagents and solutions
一一Mixed acid: add 50 ml of analytical grade concentrated sulfuric acid (GB/T625) to 250 ml of water, cool and add 12.5 g of analytical grade diammonium hydrogen citrate (HG3-1465) or ammonium citrate, 12.5 g of analytical grade tartaric acid (GB/T1294), dissolve and dilute to 500 ml with water, mix well;
一一Phenolic acid (HGB3039) : Analytical grade, 0.1% (60% ethanol) solution; - Ammonium hydroxide (GB/T631) analytical grade, concentrated and 1+1 solution; - Bicyclohexanone oxalyl dichloride, analytical grade: 0.1% solution, weigh 0.5g BCO in a 250mL beaker, add 50mL ethanol and 50mL water, heat on a water bath until dissolved, dilute to 500mL with water, mix well; - Copper standard solution, liquid A: 1mL contains 0.1mg copper. Liquid B: 1mL contains 0.01mg copper. Liquid A: weigh 0.1000g of metallic copper containing more than 99.99% copper, add 5mL 1+1 nitric acid in a 100mL beaker, heat to dissolve, wash the wall of the beaker with a small amount of water, slightly boil to remove nitrogen oxides, cool and transfer to a 1000mL volumetric flask with water, dilute to the scale, and shake well. Liquid B: Accurately pipette 10 mL of Liquid A into a 100 mL volumetric flask, dilute to scale with water, and shake well. 4.10.3 Instruments
——General laboratory instruments.
4.10.4 Determination steps
4.10.4.1 Drawing of standard curve
In seven 50 mL volumetric flasks, add 0.0, 0.5, 1.0, 1.5, 2.0, 2.5, 3.0 mL of copper standard solution B in sequence, add 20 mL of mixed acid to each, two drops of 0.1% phenolphthalein indicator, neutralize with concentrated 1+1 ammonium hydroxide to a slightly reddish color, add 10 mL of 0.1% BCO solution at 30-15°C, dilute to scale with water, and shake well. After 10 minutes of standing, take part of the solution and place it in a 2cm colorimetric blood. Take the reference solution prepared without BCO as the reference. At a wavelength of 600nm, measure the absorbance of each solution in turn. Draw a standard curve with the copper content (in mg) as the horizontal axis and the corresponding absorbance minus the reagent blank as the vertical axis. According to the above method, prepare the reference solution without BCO solution. 4.10.4.2 Determination of the sample
Take two portions of 50~100mL of the sample (depending on the copper content) and heat and evaporate them in a 250ml beaker until they smoke and dry. Add 20ml of mixed acid and heat to dissolve. If there is turbidity, filter it and then transfer it to a 50ml volumetric flask. Add two drops of 0.1% phenol crisp indicator. The following operation is carried out according to the method of drawing a standard curve. One portion does not add BCO as the sample reference solution. Subtract the absorbance of the reagent blank from the measured absorbance to find the corresponding copper content on the standard curve.
4.10.5 Calculation of results
The copper content (X) is expressed in g/L and is calculated according to formula (13): m
X=V,×1000
Wherein: ml—the amount of copper obtained from the sample absorbance curve, mg; V, the sample volume, mL.
4.11 Arsenic content
4.11.1 Principle
In the presence of potassium iodide and stannous chloride in a sulfuric acid medium, metallic zinc reacts with acid to produce new ecological hydrogen, which reacts with trivalent arsenic to form H:As gas, which is absorbed by AgDDTC-triethanolamine-chloroform solution and reacts to form a red colloidal silver solution for colorimetric determination. 4.11.2 Reagents and solutions
—— Sulfuric acid (GB/T625): analytical grade, 1+1 solution; — Tartaric acid (GB/T1294): analytical grade, 20% solution; — Potassium iodide (GB/T1272): analytical grade, 20% solution; 104
JB/T10052—1999
Stannous chloride (GB/T638): analytical grade, 40% hydrochloric acid solution, weigh 40g of stannous chloride (SnCl, ·2H) and dissolve it in 100mL 3+1 hydrochloric acid;
Arsenic-free metallic zinc (GB/T2304): 15~40 mesh honeycomb arsenic-free zinc; Silver diethylaminodithiocarbamate: analytical grade Pure, triethanolammonium: analytical grade;
-Trichloromethane (GB/T682): analytical grade; Silver diethylaminodithiocarboxylate-triethanolamine-chloroform absorption solution: weigh 0.5g of AgDDTC, dissolve it in 100ml of chloroform, add 5mL of triethanolamine, and then dilute it to 200mL with chloroform, shake to dissolve, let it stand overnight, filter it with slow filter paper into a brown bottle, and store it in a refrigerator;
-~Lead acetate (HG3-974): analytical grade, 20% solution; Lead acetate cotton: soak the absorbent cotton with 20% lead acetate solution, take it out and air it at room temperature, and keep it in a sealed container; Arsenic standard solution, solution A: 1mL contains 0.1 mg arsenic, solution B: 1 ml. Contains 0.004 mg arsenic. Liquid A: Weigh 0.1320g of high-grade pure arsenic trioxide into a 100ml beaker, add 5ml of 5% sodium hydride solution to dissolve, transfer to a 1000ml volumetric flask, dilute to the mark with water, and shake well. Liquid B: When using, accurately pipette 10mL of Liquid A into a 250mL volumetric flask, dilute to the mark with water, and shake well. 4.11.3 Instruments
Certain arsenic devices, including:
a) 100mL conical flask, used to generate hydrogen sulfide; b) connecting catheter, used to capture hydrogen sulfide and guide hydrogen arsenide into the absorption tube; c) absorption tube, used to absorb hydrogen arsenide.
General laboratory instruments
4.11.4 Determination steps
4.11.4.1 Drawing of standard curve
Add 0.0, 1.0, 2.0, 3.0, 4.0, 5.0 ml of B standard solution to six conical flasks for arsenic determination, add 9 ml of 1+1 sulfuric acid solution to each, dilute to 43 ml, add 5 ml of 20% tartaric acid solution, 5 ml of 20% potassium iodide solution, 2 ml of 40% stannous chloride solution, mix well, and place for 15 min. Plug a small amount of lead acetate cotton at the end of each connecting tube to absorb the hydrogen sulfide released during the reaction. After 15 min, add 10 ml of DDTC-trichloromethane absorption liquid to each absorption tube, quickly add 4 g of arsenic-free zinc particles to the conical flask, immediately install the instrument, plug the bottle, connect the catheter, and place for 45 min to allow the reaction to complete. Take part of the solution in a 1cm colorimetric dish, use the reagent blank solution as a reference, measure the absorbance of each solution in turn at a wavelength of 530nm, use the arsenic content (in mg) as the horizontal coordinate and the corresponding absorbance as the vertical coordinate to draw a standard curve. The standard curve must be redone every time a batch of zinc particles is changed or a new AgDDTC-chloroform solution is prepared. 4.11.4.2 Determination of the sample
Take 50ml of the sample and heat it in a 250ml beaker to evaporate and smoke until dry. Cool it slightly, add 9mL of 1+1 sulfuric acid solution, blow the wall of the cup with a small amount of water, heat and boil for 1min, cool it, move it into a conical flask for arsenic determination, control the volume to 43ml, and add 5ml of 20% tartaric acid solution. 5 ml of 20% potassium iodide solution and 2 ml of 40% stannous chloride solution, mix well, and place for 15 minutes. The following operations are performed according to the method of drawing a standard curve. The blank solution is used as a reference. The measured absorbance is checked on the standard curve to obtain the corresponding arsenic content. Perform a reagent blank test at the same time according to the above method. 4.11.5 Calculation of results
Arsenic content (X) is expressed in g/L and is calculated according to formula (14): X=vxX1000×1000
Where: m1-the amount of arsenic obtained from the sample absorbance curve, mg; (14)
Vi sample volume, ml.
5 Inspection rules
JB/T10052—1999
5.1 When preparing electrolyte for lead-acid batteries, the concentrated sulfuric acid used should meet the requirements of HG/T2692. 5.2 All water used in preparing the electrolyte for lead-acid batteries shall comply with the requirements of JB/T10053. 5.3 Each batch of lead-acid battery electrolyte must be accompanied by an inspection voucher, and its technical conditions shall comply with the technical requirements of Chapter 3. It is allowed to use other instruments to detect electrolyte impurities, but the methods specified in this standard shall be used for arbitration. 5.4 Before using the lead-acid battery electrolyte that has been stored for a long time, if there is any doubt about the quality, it should be sampled for verification. 5.5 Certain production technical records must be established for the preparation process of the lead-acid battery electrolyte. 5.6 For lead-acid battery electrolytes that have passed the inspection, each storage container should be equipped with a certificate of electrolyte quality. 6 Storage and safety
6.1 Lead-acid battery electrolytes should be stored in acid-resistant containers, and reliable measures should be taken to prevent impurities from mixing in. 6.2 The storage container of lead-acid battery electrolyte should be marked with "Lead-acid battery electrolyte" in a clearly visible position. 6.3 When using lead-acid battery electrolyte, pouring or pipe discharge method can be adopted to avoid the introduction of impurities.
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