CN107664618A - The method of testing of lignosulphonic acid sodium content in lead-acid accumulator green plate - Google Patents
The method of testing of lignosulphonic acid sodium content in lead-acid accumulator green plate Download PDFInfo
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- CN107664618A CN107664618A CN201710595976.1A CN201710595976A CN107664618A CN 107664618 A CN107664618 A CN 107664618A CN 201710595976 A CN201710595976 A CN 201710595976A CN 107664618 A CN107664618 A CN 107664618A
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N2021/3185—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry typically monochromatic or band-limited
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Abstract
The present invention relates to a kind of method of testing of lignosulphonic acid sodium content in lead-acid accumulator green plate, and by detecting sample in HAC systems, the absorbance data at 350nm draws lignosulphonic acid sodium content in lead-acid accumulator green plate.The present invention investigated using spectrophotometer come the accurate method of testing for testing out sodium lignosulfonate in green plate, and the method has the advantages of degree of accuracy is high, reproducible, simple to operate, equipment requirement is not high.
Description
Technical field
The present invention relates to a kind of method of testing of lignosulphonic acid sodium content in lead-acid accumulator green plate.
Background technology
Lead-acid battery is one of widest battery of current use range, and it developed from 19th century has lasted more than 150 so far
Year.In very long lead-acid battery evolutionary history, the lead-acid battery suitable for different purposes has been emerged in large numbers.By using different batteries
Additive, the scope of application of lead-acid battery is expanded on the premise of battery practicality is ensured.But various additives, or it is more or
The problem of its use less be present, especially from additives such as the sodium lignosulfonates in natural polymer, because it is complicated
Structure, its basic structural unit and its connected mode can only be recognized so far.
Sodium lignosulfonate is a kind of flour of the dark brown extracted from the sulfite pulp of lignin, is soluble in
Water.0.3% or so sodium lignosulfonate is added in cathode lead plaster, it becomes possible to play the work of " swelling agent " same with humic acid
With.Sodium lignosulfonate can suppress " passivation " of negative plate, the capacity and cold starting performance of battery can be played again good
Improvement result；Sodium lignosulfonate is good adhesive again, and lead plaster and grid can be made to realize and closely combine.In lignosulphonic acid
After sodium adds cathode lead plaster, negative pole overpotential of hydrogen evolution can be effectively improved, is had certain effect to suppressing self discharge.
Due to the sodium lignosulfonate advantageous effect huge to battery, so lignosulphonic acid sodium content and the uniformity of its distribution
It is exactly the problem of vast battery manufacturer is of interest.
But because sodium lignosulfonate belongs to macromolecular structure, its content can not be tested accurately, only small part document provides
Material has been reported that to carry out groping to test using ultraviolet specrophotometer, and sodium lignosulfonate has absworption peak in 290nm or so, at present not yet
The method of testing being widely recognized for having maturation occurs.Ultraviolet spectrometry degree meter equipment is high, and popularity rate is low, therefore a lot of electric power storages
Pond producer can not be tracked test to composition of the sodium lignosulfonate in green plate, can not be by the content and electricity of sodium lignosulfonate
Pond performance is excellent to be slightly associated.
The content of the invention
It is an object of the invention to provide a kind of method of testing of lignosulphonic acid sodium content in lead-acid accumulator green plate, research
Going out using spectrophotometer come the accurate method of testing for testing sodium lignosulfonate in green plate, the method has degree of accuracy height,
It is reproducible, simple to operate, the advantages of equipment requirement is low.
The method of testing of lignosulphonic acid sodium content in a kind of lead-acid accumulator green plate, by detecting sample in HAC systems
In, the absorbance data at 350nm draws lignosulphonic acid sodium content in lead-acid accumulator green plate.
The method of testing of lignosulphonic acid sodium content, detecting step are as follows in described lead-acid accumulator green plate：
(1) standard curve is drawn
(2) detection sample is prepared, step is as follows：
(1) green plate diverse location lead plaster is taken, milled processed is carried out after mixing, crosses 120 mesh sieves；
(2) testing sample accurately is weighed in beaker, add dilute hydrochloric acid solution stirring, sodium lignosulfonate is fully dissolved；
(3) solution that will be stirred in step (2), is filled into 100mL volumetric flasks, washs burning repeatedly using deionized water
Cup, makes sodium lignosulfonate fully be filled into volumetric flask；
(4) after completing filtering, mark is carried out, with deionized water constant volume, is shaken up, it is to be detected；
(3) according to test sample in HAC systems, the absorbance data at 350nm show that final sodium lignosulfonate contains
Amount.
The linear equation obtained according to standard curve is drawn：Y=a+bX, Y：Absorbance, X sample volumes, a=0.036,
B=0.9866
During sample detection, the concrete operations of step (2) add dilute accurately to weigh testing sample 2-5g in beaker
Hydrochloric acid solution (dilute hydrochloric acid solution concentration), stir 5-10 minutes.
The mass ratio of testing sample and dilute hydrochloric acid solution is 1:4.
Prepare in detection sample, step (2) accurately weighs testing sample 5g in beaker, and it is molten to add 50mL watery hydrochloric acid
Liquid, stir 5 minutes.
The plot step of standard curve：
(1) according to lead paste formula ratio in green plate, weigh corresponding monomer material and be well mixed, prepare standard curve institute
Use standard sample；
(2) according to lead paste formula ratio in green plate, sodium lignosulfonate raw material monomer is removed, weighs remaining corresponding monomer
Well mixed be used as of material removes blank solution；
(3) weigh standard sample to be placed in beaker, add 50mL deionized waters, mixing time is more than 5 minutes；
(4) solution that will be stirred in step (3), is filled into 100mL volumetric flasks, washs burning repeatedly using deionized water
Cup, makes sodium lignosulfonate fully be filled into volumetric flask；
(5) after filtering, mark is carried out, with deionized water constant volume, shakes up to obtain standard liquid stand-by；
(6) 5mL, 10mL, 20mL are pipetted respectively from standard liquid, 50mL solution carries out mark in 4 100mL capacity
Know, with deionized water constant volume, shake up to be detected；
(7) being prepared in the same method of standard liquid goes blank solution stand-by；
(8) to remove blank solution as reference, using spectrophotometer, 350nm wavelength measures standard liquid at ambient temperature
Absorbance；
(9) according to absorbance detection value, standard curve is established；
(10) linear equation is obtained according to standard curve.
The mixing time preferred 5-10 minutes of step (3).
Testing sample prepares and test：
(1) green plate diverse location lead plaster is taken, milled processed is carried out after mixing, crosses 120 mesh sieves；
(2) testing sample accurately being weighed in beaker, adding dilute hydrochloric acid solution, the mass ratio of testing sample and watery hydrochloric acid is
1:4, mixing time is more than 5 minutes；
(3) solution that will be stirred in step (2), is filled into 100mL volumetric flasks, washs burning repeatedly with deionized water
Cup, makes sodium lignosulfonate fully be filled into volumetric flask；
(4) after filtering, mark is carried out, with deionized water constant volume, shakes up detection；
(5) bring test data into linear equation and draw final lignosulphonic acid sodium content.
The mixing time preferred 5-10 minutes of step (2).
When being detected using spectrophotometer, absworption peak of the sodium lignosulfonate in HAC systems is at 350nm.
When being detected using spectrophotometer, absworption peak of the sodium lignosulfonate in HAC systems is at 350nm.
Linear equation is obtained according to standard curve.
Wherein, linear equation：Y=a+bX (1)
Y：Absorbance；X：Sample volume a=0.036b=0.9866.
Sodium lignosulfonate does not have absworption peak in visible-range, as shown in Fig. 2 carrying out test discovery using HAC systems
Occurs the absworption peak of sodium lignosulfonate at 350nm, as shown in Figure 3.It can so be surveyed with visible spectrophotometer
Examination.
Compared with prior art, the invention has the advantages that：
The method of testing of lignosulphonic acid sodium content, investigated using spectrophotometric in lead-acid accumulator green plate of the present invention
Meter carrys out the accurate method of testing for testing out sodium lignosulfonate in green plate, and the method has degree of accuracy height, reproducible, operation letter
Singly, the advantages of equipment requirement is not high.
Brief description of the drawings
Fig. 1 sodium lignosulfonates absorption curve in the range of ultraviolet light arrives；
Fig. 2 sodium lignosulfonates absorption curve in visible-range；
Fig. 3 sodium lignosulfonates absorption curve in HAC systems；
Fig. 4 standard liquid degree of fitting curves.
Embodiment
With reference to embodiment, the present invention will be further described.
Embodiment 1
The method of testing of lignosulphonic acid sodium content, step are as follows in lead-acid accumulator green plate：
First, Specification Curve of Increasing is as follows：
(1) preparation of standard liquid
(1) weigh standard specimen solution raw material monomer in table 1 and be well mixed, add 50mL deionized waters, stirred using glass bar
Mix 5 minutes；
(2) solution that will be stirred in step (1), it is filled into using filter paper and funnel in 100mL volumetric flasks, uses deionization
Water washs beaker repeatedly, sodium lignosulfonate is fully filled into volumetric flask；
(3) after completing filtering, mark is carried out, with deionized water constant volume, is shaken up stand-by；
(4) 5mL is pipetted respectively from standard sample using 10mL pipettes, 10mL, 20mL, 50mL solution is in 4
In 100mL capacity, mark is carried out, with deionized water constant volume, is shaken up to be detected；
(2) preparation of blank solution is gone
(1) weigh and blank solution raw material monomer is removed in table 1 and is well mixed, add 50mL deionized waters, use glass bar
Stirring 5 minutes；
(2) solution that will be stirred in step (1), it is filled into using filter paper and funnel in 100mL volumetric flasks, uses deionization
Water washs beaker repeatedly, sodium lignosulfonate is fully filled into volumetric flask；
(3) after completing filtering, mark is carried out, with deionized water constant volume, is shaken up stand-by；
(3) by spectrophotometer start preheating more than half an hour, to go blank as reference, at ambient temperature in 350nm
Wavelength measures standard specimen solution absorbance；Absorbance such as table 2 and the Fig. 4 of standard specimen solution in 350nm.
(4) according to spectrophotometer detected value, working curve is established.
Blank is gone to eliminate the solution of the interference of other materials in addition to detectable substance.
The standard specimen solution of table 1 and the raw material monomer composition for removing blank solution
| Composition | Standard specimen/g | Remove blank/g |
| Barium sulfate | 0.6989 | 0.7054 |
| Carbon black 220 | 0.2524 | 0.2503 |
| E sodium lignosulfonates | 0.3033 | 0 |
Absorbance of the standard specimen solution of table 2. in 350nm
| Concentration g/L | 350nm absorbances |
| 0.15 | 0.180 |
| 0.3 | 0.338 |
| 0.6 | 0.626 |
| 1.5 | 1.109 |
2nd, testing sample processing and test
(1) lead plaster is removed at green plate diverse location, is put into mortar and grinds, then sieved through 120 mesh sieve, obtained to be measured
Sample；
(2) testing sample 5.0202g is accurately weighed using assay balance in beaker, 50mL dilute hydrochloric acid solutions is added, treats
The mass ratio of test sample product and watery hydrochloric acid is 1:4, stirred 5 minutes using glass bar；
(3) solution that will be stirred in step (2), be filled into using filter paper and funnel in 100mL volumetric flasks, using go from
Sub- water washs beaker repeatedly, sodium lignosulfonate is fully filled into volumetric flask；
(4) after completing filtering, mark is carried out, with deionized water constant volume, is shaken up, it is to be detected；
(5) by spectrophotometer start preheating more than half an hour, to go blank as reference, in 350nm ripples under room temperature condition
The long prepare liquid absorbance that measures is 0.160；
(6) testing sample is brought into calibration curve equation to be calculated.
Table 3 is linear equation and result of calculation.
Wherein, linear equation：Y=a+bX Y：Absorbance X sample volume a=0.036b=0.9866 degrees of fitting：
0.9989
The linear equation of table 3 and result of calculation
。
Claims (8)
1. the method for testing of lignosulphonic acid sodium content in a kind of lead-acid accumulator green plate, it is characterised in that by detecting sample
In HAC systems, the absorbance data at 350nm draws lignosulphonic acid sodium content in lead-acid accumulator green plate.
2. the method for testing of lignosulphonic acid sodium content in lead-acid accumulator green plate according to claim 1, its feature exist
In detecting step is as follows：
(1) standard curve is drawn
(2) detection sample is prepared, step is as follows：
(1) green plate diverse location lead plaster is taken, milled processed is carried out after mixing, crosses 120 mesh sieves；
(2) testing sample accurately is weighed in beaker, add dilute hydrochloric acid solution stirring, sodium lignosulfonate is fully dissolved；
(3) solution that will be stirred in step (2), is filled into 100mL volumetric flasks, and beaker is washed repeatedly using deionized water,
Sodium lignosulfonate is set fully to be filled into volumetric flask；
(4) after completing filtering, mark is carried out, with deionized water constant volume, is shaken up, it is to be detected；
(3) according to test sample in HAC systems, the absorbance data at 350nm draws final lignosulphonic acid sodium content.
3. the method for testing of lignosulphonic acid sodium content in lead-acid accumulator green plate according to claim 1, its feature exist
In the linear equation obtained according to drafting standard curve：Y=a+bX, Y：Absorbance, X sample volumes, a=0.036, b=
0.9866。
4. the method for testing of lignosulphonic acid sodium content in lead-acid accumulator green plate according to claim 1, its feature exist
During sample detection, the concrete operations of step (2) add watery hydrochloric acid accurately to weigh testing sample 2-5g in beaker
Solution, mixing time should be greater than 5 minutes.
5. the method for testing of lignosulphonic acid sodium content in lead-acid accumulator green plate according to claim 2, its feature exist
In the mass ratio of testing sample and dilute hydrochloric acid solution is 1:4.
6. the method for testing of lignosulphonic acid sodium content in lead-acid accumulator green plate according to claim 2, its feature exist
In in preparation detection sample, step (2) accurately weighs testing sample 5g in beaker, adds 50mL dilute hydrochloric acid solutions, stirs
Mix 5 minutes.
7. the method for testing of lignosulphonic acid sodium content in lead-acid accumulator green plate according to claim 1, its feature exist
In the plot step of standard curve：
(1) according to lead paste formula ratio in green plate, weigh corresponding monomer material and be well mixed, prepare standard curve mark used
Quasi- sample；
(2) according to lead paste formula ratio in green plate, sodium lignosulfonate raw material monomer is removed, weighs remaining corresponding monomer material
Well mixed be used as removes blank solution；
(3) weigh standard sample to be placed in beaker, add 50mL deionized waters, mixing time is more than 5 minutes；
(4) solution that will be stirred in step (3), is filled into 100mL volumetric flasks, and beaker is washed repeatedly using deionized water,
Sodium lignosulfonate is set fully to be filled into volumetric flask；
(5) after filtering, mark is carried out, with deionized water constant volume, shakes up to obtain standard liquid stand-by；
(6) 5mL, 10mL, 20mL are pipetted respectively from standard liquid, 50mL solution carries out mark in 4 100mL capacity, uses
Deionized water constant volume, shake up to be detected；
(7) being prepared in the same method of standard liquid goes blank solution stand-by；
(8) to remove blank solution as reference, using spectrophotometer, 350nm wavelength measures standard liquid extinction at ambient temperature
Degree；
(9) according to absorbance detection value, standard curve is established；
(10) linear equation is obtained according to standard curve.
8. the method for testing of lignosulphonic acid sodium content in lead-acid accumulator green plate according to claim 2, its feature exist
In testing sample prepares and test：
(1) green plate diverse location lead plaster is taken, milled processed is carried out after mixing, crosses 120 mesh sieves；
(2) testing sample accurately is weighed in beaker, add dilute hydrochloric acid solution, the mass ratio of testing sample and watery hydrochloric acid is 1:4,
Stirring is more than 5 minutes；
(3) solution that will be stirred in step (2), is filled into 100mL volumetric flasks, washs beaker repeatedly with deionized water, makes
Sodium lignosulfonate is fully filled into volumetric flask；
(4) after filtering, mark is carried out, with deionized water constant volume, shakes up detection；
(5) bring test data into linear equation and draw final lignosulphonic acid sodium content.
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Cited By (2)
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| CN110715902A (en) * | 2019-08-29 | 2020-01-21 | 超威电源有限公司 | Method for detecting uniformity of positive lead paste of lead-acid storage battery |
| CN112240874A (en) * | 2020-08-07 | 2021-01-19 | 骆驼集团蓄电池研究院有限公司 | Screening method of high-temperature stable lignin for storage battery |
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