CN104237273A - Method for measuring content of 3BS (tribasic lead sulfate) and 4BS (tetrabasic lead sulfate) in cured product by X-ray diffraction internal standard method - Google Patents
Method for measuring content of 3BS (tribasic lead sulfate) and 4BS (tetrabasic lead sulfate) in cured product by X-ray diffraction internal standard method Download PDFInfo
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Abstract
The invention relates to a method for measuring the content of 3BS (tribasic lead sulfate) and 4BS (tetrabasic lead sulfate) in a cured product by an X-ray diffraction internal standard method. The method comprises the steps of carrying out qualitative treatment and content estimation on the cured product, drawing standard curves by the internal standard method, measuring the content of the cured product, adding an internal standard substance into a cured electrode plate subjected to ball grinding, and grinding again, wherein the ratio of the internal standard substance to a sample is the same as that during standard curve drawing; and measuring diffraction peaks to be detected of the internal standard substance as well as 3BS and 4BS by an X-ray diffractometer after sample preparation, recording the integrated intensity ratio of the diffraction peaks to be detected of 3BS (or 4BS) and the internal standard substance, and finding the content of 3BS and 4BS on the 3BS and 4BS standard curves. The method is convenient in qualitative analysis and accurate in quantitative analysis, and has low error less than 1%-2.5%, and therefore, the simple, rapid, accurate and effective detection method for measuring the content of 3BS and 4BS in the cured product, which is difficult to be measured accurately in the prior art, is provided.
Description
Technical field
The present invention relates to a kind of detection method, particularly relate to the method for 3BS, 4BS content in a kind of X-ray diffraction internal mark method determination solidifying lead acid battery polar plate product.
Background technology
Lead-acid battery (Lead-acid battery) electrode is made primarily of plumbous and oxide, and electrolytic solution is a kind of accumulator of sulfuric acid solution.From Frenchman Pulan spy (G.Plante) in invention lead-acid accumulator in 1859, experienced by the development course of nearly 150 years, lead-acid accumulator is in theoretical research, significant progress is obtained in product category and kind, product electric property etc., no matter be in traffic, communication, electric power, military affairs or in navigation, each economic field of aviation, lead-acid accumulator all serves indispensable vital role.In recent years, along with the acceleration of urbanization and the expansion of city scope, the magnitude of traffic flow increases severely.Although the development of the vehicles such as automobile rapidly, be subject to using the impact of the factors such as the relatively costly and rise of the oil price of price, make electric bicycle with its advantage such as spry and light, convenient, cheap, city's field depth is subject to the welcome of consumers in general at home.Lead-acid accumulator is because cost performance is high, power characteristic is good, and self discharge is little, low price, application of having got back in electric bicycle in recent years.
Lead-acid accumulator conventional curing process forms tribasic lead sulfate (3BS) by low-temperature setting, and 3BS obtains the thinner β of particle-PbO after changing into
2, make battery have higher initial capacity.And green plate can be made to form four basic lead sulphates (4BS) by hot setting, 4BS obtains the larger α of particle-PbO after changing into
2, serviceable life and the later stage capacity of battery can be improved.Form rational 3BS and 4BS proportioning, to the serviceable life of improving lead-acid accumulator, there is important effect.Because 3BS with 4BS chemical composition is similar, traditional detection method can not detect the content of 3BS, 4BS.
X-ray diffraction thing phase quantitative analysis has been widely deployed the quantitative test of crystallization phase in Materials Science and Engineering research.X-ray diffraction thing phase quantitative analysis according to being: in sample this phase content of intensity of each phase diffract spectral line increase and improve.
There is limited evidence currently of has the introduction about measuring 3BS, 4BS content method in cured product, and owing to not solving the problem of overlap of peaks, K pH-value determination pH 3BS, 4BS content using standard card valut to provide is extremely inaccurate.
Summary of the invention
The object of the invention is to solve 3BS, 4BS content method in existing mensuration cured product few, owing to not solving the problem of overlap of peaks, the extremely inaccurate defect of K pH-value determination pH 3BS, 4BS content using standard card valut to provide and a kind of method facilitating 3BS, 4BS content in simple and direct, that degree of accuracy is high X-ray diffraction internal mark method determination solidifying lead acid battery polar plate product is provided.
In order to realize above-mentioned order ground, the present invention by the following technical solutions:
Measure a method for 3BS, 4BS content in X-ray diffraction internal standard method cured product, described method comprises the qualitative of cured product and content estimation, the drafting of internal standard method typical curve, cured product assay.
In the technical program, qualitative and the content of cured product is estimated: utilize X-ray diffraction qualitative analysis, lead plaster is after hot setting, primary product is PbO, 3BS, 4BS, according to the addition of closing cream technique sulfuric acid, can calculate the total content scope of 3BS and 4BS in cured product, other a small amount of product is ignored, thus can draw PbO content range in product; The drafting of internal standard method typical curve: pbO, 3BS, 4BS that Analysis on Selecting is pure prepare testing sample, add the internal standard compound of constant ratio in testing sample, prepare serial 3BS, 4BS content different, the quaternary biased sample of the internal standard compound-PbO-3BS-4BS of PbO, internal standard compound content constant; In order to make typical curve usable range be applicable to all cured products, the minimum value of getting PbO content range is substrate; It is made fully to mix biased sample more than the mortar grinder 2h of preparation, overlapping principle the diffraction peak to be measured of internal standard compound and 3BS, 4BS in sample can not be chosen respectively again according to X-ray diffraction peak, diffraction peak to be measured is measured with X-ray diffractometer after sample preparation, record 3BS or 4BS and the integrated intensity ratio of internal standard compound diffraction peak to be measured, draw content-integrated intensity and compare typical curve;
Cured product assay: get the pole plate after solidification, be milled to particle and can cross 200 ~ 300 mesh sieve, add internal standard compound, biased sample more than mortar grinder 2h makes it fully mix, internal standard compound ratio is in the sample to which identical with ratio during Specification Curve of Increasing, measure the diffraction peak to be measured of internal standard compound and 3BS, 4BS with X-ray diffractometer after sample preparation, record 3BS(or 4BS) with the integrated intensity ratio of internal standard compound diffraction peak to be measured, on 3BS, 4BS typical curve, find the content of 3BS, 4BS respectively.
As preferably, the qualitative and content of cured product estimates it is by lead plaster after solidification, qualitative with X-ray diffraction, then calculates the content range of 3BS and 4BS in cured product according to the addition of closing cream technique sulfuric acid.
As preferably, the drafting of internal standard method typical curve is first by pure massicot, 3BS, 4BS are mixed with standard model, add internal standard compound, then use X-ray diffraction bioassay standard sample and obtain the diffraction peak to be measured of internal standard compound, 3BS and 4BS, the integrated intensity ratio of the diffraction peak to be measured of record internal standard compound, 3BS and 4BS, draws content-integrated intensity and compares typical curve.
As preferably, cured product assay is the pole plate ball milling after first getting solidification, grind after adding internal standard compound, be prepared into testing sample, then X-ray diffraction bioassay standard sample is used to obtain the diffraction peak to be measured of internal standard compound, 3BS and 4BS, the integrated intensity ratio of the diffraction peak to be measured of record internal standard compound, 3BS and 4BS, obtains 3BS, 4BS content respectively on 3BS, 4BS typical curve.
As preferably, internal standard compound is pure Si, 20% of the addition solidfied material gross mass of internal standard compound.
As preferably, when preparation standard sample and testing sample, the time of grinding is 2-4 hour.
As preferably, when preparing testing sample, being milled to pole plate grain size is 200-300 order.
As preferably, the step preparing testing sample is: get the pole plate after solidification, with an organic solvent clean surface, and being then milled to grain size is 200-300 order, adds the pure Si of internal standard compound of pole plate general assembly (TW) 20%, then grinds 2-4 hour, obtain testing sample.
As preferably, the parameter of X-ray diffraction analysis is: CuK
αradiation, pipe pressure 40kV, pipe stream 30mA, diaphragm system is DS=SS=1 °, RS=0.3mm, adopts θ-2 θ continuous sweep mode, sweep velocity 0.1 °/min.
The invention has the beneficial effects as follows that the present invention has qualitative analysis easy, quantitative test is accurate, and error 1-2.5%, provides a kind of simple and fast, accurately and effectively detection method for being difficult to 3BS, 4BS content in Accurate Determining cured product.
Accompanying drawing explanation
Fig. 1 is that in embodiment 1, the content-integrated intensity of 3BS compares typical curve.
Fig. 2 is that in embodiment 1, the content-integrated intensity of 4BS compares typical curve.
Embodiment
In order to understand the present invention further, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just in order to further illustrate the features and advantages of the present invention, instead of limiting to the claimed invention.
X-ray diffraction analysis adopts Japanese Shimadzu XRD-6100, CuK
αradiation, pipe pressure 40kV, pipe stream 30mA, diaphragm system is DS=SS=1 °, RS=0.3mm, adopts θ-2 θ continuous sweep mode, sweep velocity 0.1 °/min.
Embodiment 1
Positive plate closes cream: 1000kg lead powder and 86kg sulfuric acid, wherein, degree of oxidation of lead powder is 75%, sulfuric acid massfraction 50%.
After solidification, lead plaster composition is mainly PbO, 3BS(3PbOPbSO
4h
2and 4BS(4PbOPbSO O)
4), moisture and free lead content seldom, are ignored.
Suppose that cured product does not generate 4BS, then lead plaster composition is PbO and 3BS, and after solidification, 3BS content is 40.9%,
Suppose that cured product does not generate 3BS, then lead plaster composition is PbO and 4BS, after solidification, 4BS content is 49.7%, and in actual solidification process, cured product is generally PbO, 3BS or PbO, 3BS, 4BS, therefore in cured product, the total content of 3BS and 4BS is between 40.9% ~ 49.7%, then PbO content is between 50.3% ~ 59.1%.
The drafting of typical curve: prepare standard model with pure PbO, 3BS, 4BS, all cured products are applicable in order to make typical curve usable range, preparation PbO content is 50%, using pure Si as internal standard compound, respectively to the internal standard compound Si adding 20% in standard model, by table 1 weight proportion preparation standard model.Then grind 4h with agate mortar, make it mix.Diffracted intensity is measured, CuK with Japanese Shimadzu XRD-6100
αradiation, pipe pressure 40kV, pipe stream 30mA, diaphragm system is DS=SS=1 °, RS=0.3mm, adopt θ-2 θ continuous sweep mode, sweep velocity 0.1 °/min, measures disturbed and not overlapping 3BS(100 with X-ray diffractometer after sample preparation), 4BS(110), Si(220) diffraction peak intensity, each sample sample preparation 3 times also measures 3 times, gets the mean value of 3 diffraction peak integrated intensity ratios, records and calculate 3BS(100) or 4BS(110) and Si(220) the integrated intensity ratio of diffraction peak, draw content-integrated intensity than typical curve, see Fig. 1 and Fig. 2.
Cured product assay: get the pole plate after solidification, dry after using ethanol purge surface, be milled to particle and can cross 200 mesh sieve, add pole plate weight 20% internal standard compound Si, then grind 2h with agate mortar, make it mix.3BS(100 is measured by Specification Curve of Increasing method X-ray diffractometer) after sample preparation, 4BS(110), Si(220) diffraction peak intensity, record and calculate 3BS(100) or 4BS(110) and Si(220) the integrated intensity ratio of diffraction peak, in 3BS, 4BS, mark content typical curve being found 3BS, 4BS respectively.
Embodiment 2
Positive plate closes cream: 1000kg lead powder and 86kg sulfuric acid, wherein, degree of oxidation of lead powder is 75%, sulfuric acid massfraction 50%.
After solidification, lead plaster composition is mainly PbO, 3BS(3PbOPbSO
4h
2and 4BS(4PbOPbSO O)
4), moisture and free lead content seldom, are ignored.
Suppose that cured product does not generate 4BS, then lead plaster composition is PbO and 3BS, and after solidification, 3BS content is 40.9%,
Suppose that cured product does not generate 3BS, then lead plaster composition is PbO and 4BS, after solidification, 4BS content is 49.7%, and in actual solidification process, cured product is generally PbO, 3BS or PbO, 3BS, 4BS, therefore in cured product, the total content of 3BS and 4BS is between 40.9% ~ 49.7%, then PbO content is between 50.3% ~ 59.1%.
The drafting of typical curve: prepare standard model with pure PbO, 3BS, 4BS, all cured products are applicable in order to make typical curve usable range, preparation PbO content is 50%, using pure Si as internal standard compound, respectively to the internal standard compound Si adding 20% in standard model, by table 1 weight proportion preparation standard model.Then grind 3h with agate mortar, make it mix.Diffracted intensity is measured, CuK with Japanese Shimadzu XRD-6100
αradiation, pipe pressure 40kV, pipe stream 30mA, diaphragm system is DS=SS=1 °, RS=0.3mm, adopt θ-2 θ continuous sweep mode, sweep velocity 0.1 °/min, measure disturbed and not overlapping 3BS(100 with X-ray diffractometer after sample preparation), 4BS(110), Si(220) diffraction peak intensity, each sample sample preparation 3 times also measures 3 times, get the mean value of 3 diffraction peak integrated intensity ratios, record and calculate 3BS(100) or 4BS(110) and Si(220) the integrated intensity ratio of diffraction peak, draw content-integrated intensity and compare typical curve.
Cured product assay: get the pole plate after solidification, uses acetone clean surface, is milled to particle and can crosses 300 mesh sieve, add pole plate weight 20% internal standard compound Si, then grind 3h with agate mortar, make it mix.3BS(100 is measured by Specification Curve of Increasing method X-ray diffractometer) after sample preparation, 4BS(110), Si(220) diffraction peak intensity, record and calculate 3BS(100) or 4BS(110) and Si(220) the integrated intensity ratio of diffraction peak, in 3BS, 4BS, mark content typical curve being found 3BS, 4BS respectively.
Embodiment 3
Positive plate closes cream: 1000kg lead powder and 86kg sulfuric acid, wherein, degree of oxidation of lead powder is 75%, sulfuric acid massfraction 50%.
After solidification, lead plaster composition is mainly PbO, 3BS(3PbOPbSO
4h
2and 4BS(4PbOPbSO O)
4), moisture and free lead content seldom, are ignored.
Suppose that cured product does not generate 4BS, then lead plaster composition is PbO and 3BS, and after solidification, 3BS content is 40.9%,
Suppose that cured product does not generate 3BS, then lead plaster composition is PbO and 4BS, after solidification, 4BS content is 49.7%, and in actual solidification process, cured product is generally PbO, 3BS or PbO, 3BS, 4BS, therefore in cured product, the total content of 3BS and 4BS is between 40.9% ~ 49.7%, then PbO content is between 50.3% ~ 59.1%.
The drafting of typical curve: prepare standard model with pure PbO, 3BS, 4BS, all cured products are applicable in order to make typical curve usable range, preparation PbO content is 50%, using pure Si as internal standard compound, respectively to the internal standard compound Si adding 20% in standard model, by table 1 weight proportion preparation standard model.Then grind 2h with agate mortar, make it mix.Diffracted intensity is measured, CuK with Japanese Shimadzu XRD-6100
αradiation, pipe pressure 40kV, pipe stream 30mA, diaphragm system is DS=SS=1 °, RS=0.3mm, adopt θ-2 θ continuous sweep mode, sweep velocity 0.1 °/min, measure disturbed and not overlapping 3BS(100 with X-ray diffractometer after sample preparation), 4BS(110), Si(220) diffraction peak intensity, each sample sample preparation 3 times also measures 3 times, get the mean value of 3 diffraction peak integrated intensity ratios, record and calculate 3BS(100) or 4BS(110) and Si(220) the integrated intensity ratio of diffraction peak, draw content-integrated intensity and compare typical curve.
Cured product assay: get the pole plate after solidification, uses ethanol purge surface, is milled to particle and can crosses 250 mesh sieve, add pole plate weight 20% internal standard compound Si, then grind 4h with agate mortar, make it mix.3BS(100 is measured by Specification Curve of Increasing method X-ray diffractometer) after sample preparation, 4BS(110), Si(220) diffraction peak intensity, record and calculate 3BS(100) or 4BS(110) and Si(220) the integrated intensity ratio of diffraction peak, in 3BS, 4BS, mark content typical curve being found 3BS, 4BS respectively.
Table 1
| Sample number into spectrum | 3BS | 4BS | PbO | Si |
| 1 | 5 | 45 | 50 | 20 |
| 2 | 10 | 40 | 50 | 20 |
| 3 | 20 | 30 | 50 | 20 |
| 4 | 30 | 20 | 50 | 20 |
| 5 | 40 | 10 | 50 | 20 |
| 6 | 45 | 5 | 50 | 20 |
Composition graphs 1 and Fig. 2, prepare the verification sample that serial content is known, method for making sample is identical with during Specification Curve of Increasing with test condition, and the relative error of 3BS and 4BS assay value and design load, all at 1-2.5%, illustrates that the method may be used for the quantitative of 3BS and 4BS.
Claims (9)
1. the method for 3BS, 4BS content in X-ray diffraction internal mark method determination cured product, is characterized in that, described method comprises the qualitative of cured product and content estimation, the drafting of internal standard method typical curve, cured product assay.
2. the method for 3BS, 4BS content in a kind of X-ray diffraction internal mark method determination cured product according to claim 1, it is characterized in that, qualitative and the content of cured product estimate be by lead plaster after solidification, qualitative with X-ray diffraction, the content range of 3BS and 4BS in cured product is then calculated according to the addition of closing cream technique sulfuric acid.
3. the method for 3BS, 4BS content in a kind of X-ray diffraction internal mark method determination cured product according to claim 1, it is characterized in that, the drafting of internal standard method typical curve is first by pure massicot, 3BS, 4BS are mixed with standard model, add internal standard compound, then use X-ray diffraction bioassay standard sample and obtain the diffraction peak to be measured of internal standard compound, 3BS and 4BS, the integrated intensity ratio of the diffraction peak to be measured of record internal standard compound, 3BS and 4BS, drawing content-integrated intensity and compare typical curve.
4. the method for 3BS, 4BS content in a kind of X-ray diffraction internal mark method determination cured product according to claim 1, it is characterized in that, cured product assay is the pole plate ball milling after first getting solidification, grind after adding internal standard compound, be prepared into testing sample, then X-ray diffraction bioassay standard sample is used to obtain the diffraction peak to be measured of internal standard compound, 3BS and 4BS, the integrated intensity ratio of the diffraction peak to be measured of record internal standard compound, 3BS and 4BS, obtains 3BS, 4BS content respectively on 3BS, 4BS typical curve.
5. the method for 3BS, 4BS content in a kind of X-ray diffraction internal mark method determination cured product according to claim 1 or 2 or 3 or 4, it is characterized in that, internal standard compound is pure Si, 20% of the addition solidfied material gross mass of internal standard compound.
6. in a kind of X-ray diffraction internal mark method determination cured product according to claim 1 or 3 or 4, the method for 3BS, 4BS content, is characterized in that, when preparation standard sample and testing sample, the time of grinding is 2-4 hour.
7. in a kind of X-ray diffraction internal mark method determination cured product according to claim 1 or 3 or 4, the method for 3BS, 4BS content, is characterized in that, when preparing testing sample, being milled to pole plate grain size is 200-300 order.
8. the method for 3BS, 4BS content in a kind of X-ray diffraction internal mark method determination cured product according to claim 3, it is characterized in that, the step preparing testing sample is: get the pole plate being after solidification, with an organic solvent clean surface, then being milled to grain size is 200-300 order, add the pure Si of internal standard compound of pole plate being general assembly (TW) 20%, then grind 2-4 hour, obtain testing sample.
9. the method for 3BS, 4BS content in a kind of X-ray diffraction internal mark method determination cured product according to claim 1 or 2 or 3 or 4, it is characterized in that, the parameter of X-ray diffraction analysis is: CuK
αradiation, pipe pressure 40kV, pipe stream 30mA, diaphragm system is DS=SS=1 °, RS=0.3mm, adopts θ-2 θ continuous sweep mode, sweep velocity 0.1 °/min.
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