CN107290292A - The detection method of additive dispersion effect in lead plaster in a kind of lead-acid accumulator - Google Patents
The detection method of additive dispersion effect in lead plaster in a kind of lead-acid accumulator Download PDFInfo
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Abstract
The present invention relates to Lead-acid Battery Technology field, specifically disclose a kind of detection method of additive dispersion effect in lead plaster in lead-acid accumulator, lead plaster sample preparation is gathered into solution, through atomic absorption spectrometry liquor B a contents, contained Ba quality N in the lead plaster sample of unit of account quality, then the N of all lead plaster samples average value M is calculated, standard deviation S, standard deviation rate s is calculated again, the scattered uniformity coefficient of additive is reflected by standard deviation rate s, standard deviation rate is more than setting value, and then the sampling pole plate is undesirable, standard deviation rate is less than or equal to setting value, and then the sampling pole plate meets the requirements, different sampling pole plates is when especially standard deviation rate is respectively less than setting value, the smaller then additive of standard deviation rate is more dispersed, so as to accurate, intuitively, quickly determine dispersion effect of the additive in lead plaster, test basis for estimation is provided to improve additive dispersing technology.
Description
Technical field
Invention is related to Lead-acid Battery Technology field, and in particular to additive disperses in lead plaster in a kind of lead-acid accumulator
The detection method of effect.
Background technology
Lead-acid accumulator is a kind of performance stabilization, safe charge power supply, and its production process includes lead powder manufacture, plate
Grid manufacture, lead plaster and system, pole plate are coated, polar plate solidification is dried, pole plate is melted into and battery assemble etc. process.Additive is that plumbic acid stores
The important pole plate auxiliary material of battery, including barium sulfate, sodium lignosulfonate etc., additive is added in lead plaster simultaneously in lead plaster and process processed
It is coated on green plate.The degree of being uniformly dispersed of additive decides the stability of battery quality, and whether additive is uniformly dispersed
Not only show the quality height of lead plaster in lead-acid accumulator, existing additive dispersing technology is also reflected to a certain extent is
It is no to need to improve.But existing lead plaster and point for being the apparent density of lead plaster and additive can not being accurately reflected of process processed detection
Dissipate effect.Therefore it is highly desirable to set up a kind of detection method of accurate evaluation additive dispersion effect, to improve lead acid storage battery
The stability in pond.
The content of the invention
For lead plaster pole plate in lead-acid accumulator additive dispersion effect can not accurate and effective detection evaluate the problem of, this
The purpose of invention is to provide a kind of detection method of additive dispersion effect in lead plaster in lead-acid accumulator, can be accurate, straight
See, quickly determine dispersion effect of the additive in lead plaster, be favorably improved the stability of lead-acid accumulator, also add to improve
Plus agent dispersing technology provides test basis for estimation.
The present invention provides following technical scheme：
The detection method of additive dispersion effect in lead plaster, comprises the following steps in a kind of lead-acid accumulator：
(1) test specimens are prepared, barium sulfate BaSO will be contained4Additive be added in lead powder and be uniformly mixed and made into lead plaster, by lead
Cream is coated in solidification on green plate and sampling pole plate is made, and remembers sample position in sampling pole plate subscript and gathers lead plaster sample；
(2) test fluid is prepared, sulfuric acid H is dissolved in after lead plaster sample is calcined2SO4Test is made in solution and ultrafiltration, constant volume filtrate
Liquid；
(3) titer is prepared, the barium ions Ba that the theoretical content according to barium Ba in lead plaster is calculated2+Concentration c prepare 8~15
The BaSO of concentration gradient4Standard liquid, makes Ba in test specimens2+Concentration be in BaSO4In the range of the concentration gradient of standard liquid；
(4) by BaSO4Standard liquid is placed on Atomic Absorption Spectrometer the BaSO for testing various concentrations4The absorbance of standard liquid
λ, absorbance λ-Ba are obtained according to test result2+Concentration equation of linear regression；
(5) test fluid of different lead plaster sample preparations is respectively placed in test on Atomic Absorption Spectrometer and obtains absorbance λ, then
Equation of linear regression in step (4) calculates Ba in test fluid2+Concentration C；
(6) Ba in step (5)2+Concentration C, the lead plaster of the Mass Calculation unit mass of test fluid volume and lead plaster sample
Contained Ba quality N mg/g in sample；
(7) the average value M and standard deviation S of contained Ba quality on same sampling pole plate, wherein M=(∑ N)/n, S=are calculated
[(∑(N-M)2)/(n-1)]1/2, n is sample position number；
(8) and then standard deviation rate s, s=S/M × 100%, standard of comparison deviation ratio and setting value, if standard deviation rate are calculated
More than setting value, then the sampling pole plate is undesirable, and the sampling pole plate meets if standard deviation rate is less than or equal to setting value
It is required that；
(9) the s values of different sampling pole plates are calculated respectively according to above-mentioned steps, the scattered of the additive on not plates of similar polarity is compared by s
The smaller then distribution of additives of effect, wherein s is more uniform, and s is more big, and then distribution of additives is more scattered.
The detection method of additive dispersion effect in lead plaster in the lead-acid accumulator of the present invention, is sampled by quantitative calculate
Diverse location Ba content distribution and then the distribution situation of additive is accurately reflected out on pole plate, the lead on green plate is gathered first
Cream sample preparation is into solution, then ultrafiltration and constant volume filtrate, through the Ba contents in atomic absorption spectrometry filtrate, Jin Erji
Ba contained in the lead plaster sample of unit mass quality N is calculated, the N of all lead plaster samples average value M, standard is then calculated
Poor S, then standard deviation rate s is calculated, can be accurate by standard deviation rate s because the quality of every part of lead plaster sample has differences
Really reflect the scattered uniformity coefficient of additive.For one piece of sampling pole plate, the sampling if standard deviation rate is more than setting value
Pole plate is undesirable, and the sampling pole plate meets the requirements if standard deviation rate is less than or equal to setting value, is taken for different
Sample pole plate, when especially its standard deviation rate is respectively less than setting value, the smaller then additive of standard deviation rate is more dispersed, and then
Reflect that the adding technology that the sampling pole plate is used is more reasonable.The detection method is applied to contain BaSO4Additive, also fit
For quantitatively adding BaSO into additive4Then detect, can accurate, directly perceived, quickly determine point of the additive in lead plaster
Effect is dissipated, the stability of lead-acid accumulator is favorably improved, also test basis for estimation is provided to improve additive dispersing technology.
Improved as one kind of the inventive method, the method for step (1) acceptance of the bid note sample position is as follows：On sampling pole plate
Make two diagonal, grown using the midpoint of two cornerwise intersection points and the summit line of sampling pole plate as the center of circle, with cornerwise 1/8
Make to justify for radius, circle is sample position with cornerwise two intersection points and two cornerwise intersection points, each samples pole plate
On have 9 sample position.Large range of sampling so can be covered on sampling pole plate, it is ensured that testing result is accurately reflected
Go out distribution situation of the additive in lead plaster.
Being improved as one kind of the inventive method, calcining heat is 600~700 DEG C in step (2), calcination time is 60~
90 minutes, H2SO4The concentration of solution is 2~4mol/L, and addition volume is 50~80mL.It is organic in removal sample by calcining
Thing, combined moisture, remove detection interference.
Improved as one kind of the inventive method, cellulose acetate film or aperture of the filter membrane used in ultrafiltration for 0.45 μm of aperture
0.45 μm of polyvinylidene fluoride film.Adsorbance to the material in solution is minimum, it is ensured that detection is accurate.
Improved as one kind of the inventive method, the BaSO in step (3)4In the concentration of the centre of standard liquid or two
Between the Ba that calculates of the average value of concentration and the theoretical content of Ba in lead plaster2+Concentration c deviation be ± 5%.Work as BaSO4Standard
When the number of the gradient concentration of solution is odd number, BaSO4Ba theoretical content meter in the concentration and lead plaster of the centre of standard liquid
The Ba of calculation2+Concentration c deviation be ± 5%, work as BaSO4When the number of the gradient concentration of standard liquid is even number, BaSO4Standard
The Ba that Ba theoretical content is calculated in the concentration and lead plaster of the centre of solution2+Concentration c deviation be ± 5%, such lead plaster sample
Ba concentration is as far as possible in BaSO in product4In the range of the gradient concentration of solution, detection is improved accurate.Ba reason wherein in lead plaster
By the Ba of cubage2+Concentration c calculated through following methods：
C=A × w%/V, wherein A represent the quality of lead plaster sample, w% represent Ba with the mass fraction in the lead plaster being made, v
Represent the constant volume of test fluid.
Improved as one kind of the inventive method, the setting value in step (8) is determined by following methods, takes 100~200 pieces
The green plate of up-to-standard coating lead plaster, calculates the s of every piece of green plate, so respectively according to the process of step (1)~step (8)
S average value as setting value is sought afterwards.The distribution of additives effect sampled in pole plate is weighed by setting setting value, is added to improve
Plus agent dispersing technology provides test basis for estimation.
Improved as one kind of the inventive method, Atomic Absorption Spectrometer used is graphite furnace atomic absorption spectrophotometer.Stone
Black stove Atomic Absorption Spectrometer sensitivity is high, and test limit is up to 10-6~10-14, 10 can be measured-13The g/ml orders of magnitude, can accurate quantitative analysis
Ba contents, are particularly suitable for use in and micro BaSO are added into additive4Detected.
Improved as one kind of the inventive method, the detection parameter of graphite furnace atomic absorption spectrophotometer is as follows：Wavelength
455.4nm, slit width 0.5nm, lamp current 10mA, burner height 8mm, heating schedule is：25 DEG C~120 DEG C, heating speed
10 DEG C/s of rate, keeps 40s；120 DEG C~1700 DEG C, 10 DEG C/s of heating rate keeps 30s；1700 DEG C~2700 DEG C, heating rate
30 DEG C/s, keep 5s；2700 DEG C~2800 DEG C, 10 DEG C/s of heating rate keeps 5s.Detection process is set preferable noise occur
Than, ambient interferences are discharged, and Ba absorbance is maximum.
Beneficial effects of the present invention are as follows
The detection method of additive dispersion effect in lead plaster in the lead-acid accumulator of the present invention, pole plate is sampled by quantitative calculate
Upper diverse location Ba content distribution and then the distribution situation for accurately reflecting out additive, accurate, directly perceived, quick can determine and add
Plus dispersion effect of the agent in lead plaster, by setting the distribution of additives situation on setting value judge monolithic sampling pole plate, pass through
Standard deviation rate judge it is different sampling pole plates distribution of additives situations, be favorably improved the stability of lead-acid accumulator, also for
Improve additive dispersing technology and test basis for estimation is provided.
Brief description of the drawings
Fig. 1 is the sample position mark for sampling pole plate.
In figure：1st, sample pole plate, 11, sample position 1., 12, sample position 2., 13, sample position 3., 14, sample position
4., 15, sample position 5., 16, sample position 6., 17, sample position 7., 18, sample position 8., 19, sample position 9..
Embodiment
Just the embodiment of the present invention is described further below.
Unless otherwise instructed, the raw material employed in the present invention is commercially available or commonly used in the art, such as
Without special instruction, the method in following embodiments is the conventional method of this area.
The preferred graphite furnace atomic absorption spectrophotometer of Atomic Absorption Spectrometer, graphite furnace atomic absorption spectrophotometer detection preferably
Parameter is as follows：Wavelength 455.4nm, slit width 0.5nm, lamp current 10mA, burner height 8mm, heating schedule is：25 DEG C~
120 DEG C, 10 DEG C/s of heating rate keeps 40s；120 DEG C~1700 DEG C, 10 DEG C/s of heating rate keeps 30s；1700 DEG C~
2700 DEG C, 30 DEG C/s of heating rate keeps 5s；2700 DEG C~2800 DEG C, 10 DEG C/s of heating rate keeps 5s.
Embodiment 1
The detection method of additive dispersion effect in lead plaster, comprises the following steps in a kind of lead-acid accumulator：
(1) test specimens are prepared, barium sulfate BaSO will be contained4Additive be added in lead powder and be uniformly mixed and made into lead plaster, by lead
Cream is coated on green plate solidification and sampling pole plate is made, sampling pole plate subscript note sample position and gather lead plaster sample 1 ±
0.5mg, preferably marks the method for sample position as follows：As shown in figure 1, making two diagonal on sampling pole plate 1, with two pairs
The midpoint of summit line of the intersection point of linea angulata with sampling pole plate is made to justify for the center of circle, with cornerwise 1/8 a length of radius, round and diagonal
Two intersection points and two cornerwise intersection points of line are sample position, and 9 sample position are had on each sampling pole plate,
Respectively sample position 1. 11, sample position 2. 12, sample position 3. 13, sample position 4. 14, sample position 5. 15, sampling position
Put 6. 16, sample position 7. 17, sample position 8. 18, sample position 9. 19；
(2) test fluid is prepared, 2mol/L sulfuric acid H will be completely dissolved in after the calcining 60 minutes of 600 DEG C of lead plaster sample2SO4Solution
In 50mL, then filtering is precipitated and ultrafiltrate, and constant volume filtrate to 1000mL obtains test fluid, and filter membrane used in ultrafiltration is aperture
0.45 μm of cellulose acetate film；
(3) titer is prepared, the barium ions Ba that the theoretical content according to barium Ba in lead plaster is calculated2+Concentration c prepare 8 concentration
The BaSO of gradient4Standard liquid, makes Ba in test specimens2+Concentration be in BaSO4In the range of the concentration gradient of standard liquid, wherein
C=A × w%/V, A represent the quality of lead plaster sample, w% represent Ba with the mass fraction in the lead plaster being made, v represents test
The constant volume of liquid, preferably BaSO4Ba theoretical content meter in the average value and lead plaster of the concentration of two centres of standard liquid
The Ba of calculation2+Concentration c deviation be ± 5%；
(4) by BaSO4Standard liquid is placed on Atomic Absorption Spectrometer the BaSO for testing various concentrations4The absorbance of standard liquid
λ, absorbance λ-Ba are obtained according to test result2+Concentration equation of linear regression, goodness of fit R2≥0.995；
(5) test fluid of different lead plaster sample preparations is respectively placed in test on Atomic Absorption Spectrometer and obtains absorbance λ, then
Equation of linear regression in step (4) calculates Ba in test fluid2+Concentration C；
(6) Ba in step (5)2+Concentration C, the lead plaster of the Mass Calculation unit mass of test fluid volume and lead plaster sample
Contained Ba quality N mg/g in sample；
(7) the average value M and standard deviation S of contained Ba quality on same sampling pole plate, wherein M=(∑ N)/n, S=are calculated
[(∑(N-M)2)/(n-1)]1/2, n is sample position number, wherein n=9；
(8) and then standard deviation rate s, s=S/M × 100%, standard of comparison deviation ratio and setting value, if standard deviation rate are calculated
More than setting value, then the sampling pole plate is undesirable, and the sampling pole plate meets if standard deviation rate is less than or equal to setting value
It is required that, wherein setting value is determined by following methods, the green plate of 100 pieces of up-to-standard coating lead plasters is taken, by step (1)~step
Suddenly the process of (8) calculates the s of every piece of green plate respectively, then seeks s average value as setting value, setting value is 5%；
(9) the s values of different sampling pole plates are calculated respectively according to above-mentioned steps, the scattered of the additive on not plates of similar polarity is compared by s
The smaller then distribution of additives of effect, wherein s is more uniform, and s is more big, and then distribution of additives is more scattered.
Optional 5 pieces of samplings pole plate, the result obtained through above-mentioned processing method is as shown in table 1 below.
Table 1
From upper table 1 as can be seen that compared with setting value 5%, each sampling pole plate meets the requirements in addition to pole plate 5 is sampled, simultaneously
The s values for sampling pole plate 2 are minimum, and additive degree of scatter is most uniform, behind be followed successively by and sample pole plate 4,1,3.
Embodiment 2
The detection method of additive dispersion effect in lead plaster, comprises the following steps in a kind of lead-acid accumulator：
(1) test specimens are prepared, barium sulfate BaSO will be contained4Additive be added in lead powder and be uniformly mixed and made into lead plaster, by lead
Cream is coated on green plate solidification and sampling pole plate is made, sampling pole plate subscript note sample position and gather lead plaster sample 1 ±
0.5mg, preferably marks the method for sample position as follows：As shown in figure 1, making two diagonal on sampling pole plate 1, with two pairs
The midpoint of summit line of the intersection point of linea angulata with sampling pole plate is made to justify for the center of circle, with cornerwise 1/8 a length of radius, round and diagonal
Two intersection points and two cornerwise intersection points of line are sample position, and 9 sample position are had on each sampling pole plate,
Respectively sample position 1. 11, sample position 2. 12, sample position 3. 13, sample position 4. 14, sample position 5. 15, sampling position
Put 6. 16, sample position 7. 17, sample position 8. 18, sample position 9. 19；
(2) test fluid is prepared, 3mol/L sulfuric acid H will be completely dissolved in after the calcining 75 minutes of 650 DEG C of lead plaster sample2SO4Solution
In 65mL, then filtering is precipitated and ultrafiltrate, and constant volume filtrate to 1000mL obtains test fluid, and filter membrane used in ultrafiltration is aperture
0.45 μm of polyvinylidene fluoride film；
(3) titer is prepared, the barium ions Ba that the theoretical content according to barium Ba in lead plaster is calculated2+Concentration c prepare 12 concentration
The BaSO of gradient4Standard liquid, makes Ba in test specimens2+Concentration be in BaSO4In the range of the concentration gradient of standard liquid, wherein
C=A × w%/V, A represent the quality of lead plaster sample, w% represent Ba with the mass fraction in the lead plaster being made, v represents test
The constant volume of liquid, preferably BaSO4Ba theoretical content is calculated in the average value and lead plaster of the concentration of two centres of standard liquid
Ba2+Concentration c deviation be ± 5%；
(4) by BaSO4Standard liquid is placed on Atomic Absorption Spectrometer the BaSO for testing various concentrations4The absorbance of standard liquid
λ, absorbance λ-Ba are obtained according to test result2+Concentration equation of linear regression, goodness of fit R2≥0.995；
(5) test fluid of different lead plaster sample preparations is respectively placed in test on Atomic Absorption Spectrometer and obtains absorbance λ, then
Equation of linear regression in step (4) calculates Ba in test fluid2+Concentration C；
(6) Ba in step (5)2+Concentration C, the lead plaster of the Mass Calculation unit mass of test fluid volume and lead plaster sample
Contained Ba quality N mg/g in sample；
(7) the average value M and standard deviation S of contained Ba quality on same sampling pole plate, wherein M=(∑ N)/n, S=are calculated
[(∑(N-M)2)/(n-1)]1/2, n is sample position number, wherein n=9；
(8) and then standard deviation rate s, s=S/M × 100%, standard of comparison deviation ratio and setting value, if standard deviation rate are calculated
More than setting value, then the sampling pole plate is undesirable, and the sampling pole plate meets if standard deviation rate is less than or equal to setting value
It is required that, wherein setting value is determined by following methods, the green plate of 150 pieces of up-to-standard coating lead plasters is taken, by step (1)~step
Suddenly the process of (8) calculates the s of every piece of green plate respectively, then seeks s average value as setting value, setting value is 5%；
(9) the s values of different sampling pole plates are calculated respectively according to above-mentioned steps, the scattered of the additive on not plates of similar polarity is compared by s
The smaller then distribution of additives of effect, wherein s is more uniform, and s is more big, and then distribution of additives is more scattered.
Optional 5 pieces of samplings pole plate, the result obtained through above-mentioned processing method is as shown in table 2 below.
Table 2
From upper table 2 as can be seen that sampling pole plate 6,7,8,9,10 s values respectively 8.306%, 3.617%, 4.567%,
5.052%th, 4.966%, compared with setting value 5%, sampling pole plate 6 and 9 undesirable, the additive degree that is uniformly dispersed is poor,
Additive degree of scatter is more uniform in sampling pole plate 7,8,10, simultaneously because the s values of sampling pole plate 7 are minimum, therefore sampling pole plate 7
Middle additive is scattered most uniform.
Step (2)~step (8) that test fluid obtained by 5 pieces of sampling pole plates in embodiment 1 is passed through in embodiment 2 in addition
Result after processing is as shown in table 2-1.
Table 2-1
As can be seen that sampling pole plate 5 does not meet the requirement of setting value 5% from table 2-1, additive point in pole plate 2 is then sampled
Scattered degree is the most uniform, behind be followed successively by sampling pole plate 4,1,3, it is identical with the analytical conclusions in embodiment 1, show detection side
Method has good reappearance.
Embodiment 3
The detection method of additive dispersion effect in lead plaster, comprises the following steps in a kind of lead-acid accumulator：
(1) test specimens are prepared, barium sulfate BaSO will be contained4Additive be added in lead powder and be uniformly mixed and made into lead plaster, by lead
Cream is coated on green plate solidification and sampling pole plate is made, sampling pole plate subscript note sample position and gather lead plaster sample 1 ±
0.5mg, preferably marks the method for sample position as follows：As shown in figure 1, making two diagonal on sampling pole plate 1, with two pairs
The midpoint of summit line of the intersection point of linea angulata with sampling pole plate is made to justify for the center of circle, with cornerwise 1/8 a length of radius, round and diagonal
Two intersection points and two cornerwise intersection points of line are sample position, and 9 sample position are had on each sampling pole plate,
Respectively sample position 1. 11, sample position 2. 12, sample position 3. 13, sample position 4. 14, sample position 5. 15, sampling position
Put 6. 16, sample position 7. 17, sample position 8. 18, sample position 9. 19；
(2) test fluid is prepared, 4mol/L sulfuric acid H will be completely dissolved in after the calcining 90 minutes of 700 DEG C of lead plaster sample2SO4Solution
In 80mL, then filtering is precipitated and ultrafiltrate, and constant volume filtrate to 1000mL obtains test fluid, and filter membrane used in ultrafiltration is aperture
0.45 μm of cellulose acetate film；
(3) titer is prepared, the barium ions Ba that the theoretical content according to barium Ba in lead plaster is calculated2+Concentration c prepare 15 concentration
The BaSO of gradient4Standard liquid, is followed successively by, and makes Ba in test specimens2+Concentration be in BaSO4The concentration gradient scope of standard liquid
Interior, wherein c=A × w%/V, A represents the quality of lead plaster sample, w% represent Ba with the mass fraction in the lead plaster being made, v
Represent the constant volume of test fluid, preferably BaSO4Ba theoretical content is calculated in the concentration and lead plaster of the centre of standard liquid
Ba2+Concentration c deviation be ± 5%；
(4) by BaSO4Standard liquid is placed on Atomic Absorption Spectrometer the BaSO for testing various concentrations4The absorbance of standard liquid
λ, absorbance λ-Ba are obtained according to test result2+Concentration equation of linear regression, goodness of fit R2≥0.995；
(5) test fluid of different lead plaster sample preparations is respectively placed in test on Atomic Absorption Spectrometer and obtains absorbance λ, then
Equation of linear regression in step (4) calculates Ba in test fluid2+Concentration C；
(6) Ba in step (5)2+Concentration C, the lead plaster of the Mass Calculation unit mass of test fluid volume and lead plaster sample
Contained Ba quality N mg/g in sample；
(7) the average value M and standard deviation S of contained Ba quality on same sampling pole plate, wherein M=(∑ N)/n, S=are calculated
[(∑(N-M)2)/(n-1)]1/2, n is sample position number, wherein n=9；
(8) and then standard deviation rate s, s=S/M × 100%, standard of comparison deviation ratio and setting value, if standard deviation rate are calculated
More than setting value, then the sampling pole plate is undesirable, and the sampling pole plate meets if standard deviation rate is less than or equal to setting value
It is required that, wherein setting value is determined by following methods, the green plate of 200 pieces of up-to-standard coating lead plasters is taken, by step (1)~step
Suddenly the process of (8) calculates the s of every piece of green plate respectively, then seeks s average value as setting value, setting value is 5%；
(9) the s values of different sampling pole plates are calculated respectively according to above-mentioned steps, the scattered of the additive on not plates of similar polarity is compared by s
The smaller then distribution of additives of effect, wherein s is more uniform, and s is more big, and then distribution of additives is more scattered.
Optional 5 pieces of samplings pole plate, the result obtained through above-mentioned processing method is as shown in table 3 below.
Table 3
As can be seen from the above table, sampling pole plate 11,12,13,14,15 s values respectively 3.700%, 7.511%,
2.965%th, 5.580%, 6.648%, compared with setting value 5%, sampling pole plate 12,14,15 is undesirable, and additive disperses
Uniformity coefficient is poor, and the additive degree of scatter for sampling pole plate 11,13 is more uniform, simultaneously because the s values of sampling pole plate 13 are most
It is small, show that additive degree of scatter is most uniform in sampling pole plate 3.
Step (2)~step (8) that test fluid obtained by 5 pieces of sampling pole plates in embodiment 1 is passed through in embodiment 3 in addition
Result after processing is as shown in table 3-1.
Table 3-1
As can be seen that sampling pole plate 5, which does not meet additive in the requirement of setting value 5%, sampling pole plate 2, disperses journey from table 3-1
Degree it is the most uniform, behind be followed successively by sampling pole plate 4,1,3, it is identical with the analytical conclusions in embodiment 1, performance output detection method tool
There is good reappearance.
Claims (8)
1. the detection method of additive dispersion effect in lead plaster, comprises the following steps in a kind of lead-acid accumulator：
（1）Test specimens are prepared, barium sulfate BaSO will be contained4Additive be added in lead powder and be uniformly mixed and made into lead plaster, by lead plaster
It is coated in solidification on green plate and sampling pole plate is made, remembers sample position in sampling pole plate subscript and gather lead plaster sample；
（2）Test fluid is prepared, sulfuric acid H is dissolved in after lead plaster sample is calcined2SO4Test is made in solution and ultrafiltration, constant volume filtrate
Liquid；
（3）Titer is prepared, the barium ions Ba that the theoretical content according to barium Ba in lead plaster is calculated2+Concentration c prepare 8~15 it is dense
Spend the BaSO of gradient4Standard liquid, makes Ba in test specimens2+Concentration be in BaSO4In the range of the concentration gradient of standard liquid；
（4）By BaSO4Standard liquid is placed on Atomic Absorption Spectrometer the BaSO for testing various concentrations4The absorbance of standard liquid
λ, absorbance λ-Ba are obtained according to test result2+Concentration equation of linear regression；
（5）The test fluid of different lead plaster sample preparations is respectively placed in test on Atomic Absorption Spectrometer and obtains absorbance λ, then
According to step（4）In equation of linear regression calculate Ba in test fluid2+Concentration C；
（6）By step（5）Middle Ba2+Concentration C, the lead plaster sample of the Mass Calculation unit mass of test fluid volume and lead plaster sample
Contained Ba quality N mg/g in product；
（7）The average value M and standard deviation S of contained Ba quality on the same sampling pole plate of calculating, wherein M=(∑ N)/n, S=
[(∑(N-M)2)/(n-1)]1/2, n is sample position number；
（8）Then standard deviation rate s, s=S/M × 100%, standard of comparison deviation ratio and setting value are calculated, if standard deviation rate is big
In setting value, then the sampling pole plate is undesirable, and the sampling pole plate is conformed to if standard deviation rate is less than or equal to setting value
Ask；
（9）Calculate the s values of different sampling pole plates respectively according to above-mentioned steps, the scattered of the additive on not plates of similar polarity is compared by s
The smaller then distribution of additives of effect, wherein s is more uniform, and s is more big, and then distribution of additives is more scattered.
2. the detection method of additive dispersion effect in lead plaster, its feature in lead-acid accumulator according to claim 1
It is, step（1）The method of acceptance of the bid note sample position is as follows：Make two diagonal on sampling pole plate, with two cornerwise friendships
The midpoint of point and the summit line of sampling pole plate is made to justify for the center of circle, with cornerwise 1/8 a length of radius, circle and cornerwise two
Intersection point and two cornerwise intersection points are sample position, and 9 sample position are had on each sampling pole plate.
3. the detection method of additive dispersion effect in lead plaster, its feature in lead-acid accumulator according to claim 1
It is, step（2）Middle calcining heat is 600~700 DEG C, and calcination time is 60~90 minutes, H2SO4The concentration of solution is 2~4
Mol/L, addition volume is 50~80 mL.
4. the detection method of additive dispersion effect in lead plaster, its feature in lead-acid accumulator according to claim 3
It is, filter membrane used in ultrafiltration is the cellulose acetate film in 0.45 μm of aperture or the polyvinylidene fluoride film in 0.45 μm of aperture.
5. the detection method of additive dispersion effect in lead plaster, its feature in lead-acid accumulator according to claim 1
It is, step（3）In BaSO4Ba in the average value and lead plaster of the concentration of the centre of standard liquid or the concentration of two centres
The Ba that theoretical content is calculated2+Concentration c deviation be ± 5%.
6. the detection method of additive dispersion effect in lead plaster, its feature in lead-acid accumulator according to claim 1
It is, step（8）In setting value determined by following methods, take the green plates of 100~200 pieces of up-to-standard coating lead plasters,
According to step（1）~step（8）Process calculate the s of every piece of green plate respectively, then seek s average value as setting value.
7. according to the detection method of additive dispersion effect in lead plaster in any described lead-acid accumulator of claim 1 to 6,
Characterized in that, Atomic Absorption Spectrometer used is graphite furnace atomic absorption spectrophotometer.
8. the detection method of additive dispersion effect in lead plaster, its feature in lead-acid accumulator according to claim 7
It is, the detection parameter of graphite furnace atomic absorption spectrophotometer is as follows：The nm of wavelength 455.4, the nm of slit width 0.5, lamp current 10
MA, the mm of burner height 8, heating schedule is：25 DEG C~120 DEG C, 10 DEG C/s of heating rate keeps 40 s；120 DEG C~
1700 DEG C, 10 DEG C/s of heating rate keeps 30 s；1700 DEG C~2700 DEG C, 30 DEG C/s of heating rate keeps 5 s；
2700 DEG C~2800 DEG C, 10 DEG C/s of heating rate keeps 5 s.
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