CN105758684A - Preparation method of moisture test sample and test method - Google Patents
Preparation method of moisture test sample and test method Download PDFInfo
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- CN105758684A CN105758684A CN201610152300.0A CN201610152300A CN105758684A CN 105758684 A CN105758684 A CN 105758684A CN 201610152300 A CN201610152300 A CN 201610152300A CN 105758684 A CN105758684 A CN 105758684A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/42—Measuring deposition or liberation of materials from an electrolyte; Coulometry, i.e. measuring coulomb-equivalent of material in an electrolyte
- G01N27/44—Measuring deposition or liberation of materials from an electrolyte; Coulometry, i.e. measuring coulomb-equivalent of material in an electrolyte using electrolysis to generate a reagent, e.g. for titration
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Abstract
The invention relates to the field of moisture analysis and discloses a preparation method of a moisture test sample and a test method. The preparation method of the moisture test sample comprises steps as follows: a sample is added to a sample preparation bottle under a sample preparation condition, and the sample preparation bottle is sealed and serves as a test sample; alternatively, the sample preparation bottle is directly sealed under a sample preparation condition and serves as a blank sample, wherein the sample preparation condition comprises basically constant moisture content. The test method of the moisture test sample comprises steps as follows: the moisture detection sample is prepared with the preparation method, and the obtained moisture detection sample is subjected to moisture detection with a Karl-fischer potentiometric titration method. The preparation method of the moisture test sample and the test method have the advantages that the cost is reduced, the test data errors are reduced, the work efficiency is improved, and the service life of a moisture meter is prolonged.
Description
Technical field
The present invention relates to water analysis field, in particular it relates to the preparation method of a kind of moisture measurement sample and detection method.
Background technology
One of quantitative analysis elementary item being listed in all kinds of material physico-chemical analysis of progressive moisture along with the development of scientific research and production technology, as an important quality index of all kinds of materials.The different requirements measuring moisture are proposed according to the different in moisture content in multi-form sample.Determination of water can be that industrial control is analyzed, it is also possible to is the quality signing of industrial and agricultural products；Moisture can be measured from the product becoming ton meter and only can also carry out water analysis with number microlitre test solution in the lab；Can be the water content constant water analysis that reaches a few percent to tens, it is also possible to be the water content trace water analysis etc. that is only less than 1/1000000th.
In the test process of powder body moisture, it is common to use be that the combination of the logical cassette cooker 860 of Switzerland ten thousand and KF831 Moisture Meter carries out testing (karl Fischer potentiometric titration).In order to ensure the accuracy of data, answer the suggestion of the logical producer test expert of Switzerland ten thousand, it is necessary to before every day test sample, first prepare the blank sample on the same day.In test result, it is desirable to the absolute water content meansigma methods of blank sample is less than 10 μ g, if more than 10 μ g, then need to get rid of abnormal cause, the standby blank sample of brand-new of laying equal stress on, but prepare blank sample in atmosphere and be easy to so that absolute water content meansigma methods is more than 10 μ g.Additionally, due to need to prepare in real time blank sample, causing that in preparation process, moisture is not easily controlled, data fluctuations is bigger.These factors are easy for causing in test process test, and data are not accurate enough, abnormal conditions increase, lose time, waste material and increase the weight of the negative consequence such as load of Moisture Meter.Therefore, the accuracy of said method and economy are unsatisfactory.
Summary of the invention
It is an object of the invention to overcome in existing technique need the blank sample of preparation every day to lose time, waste material, the test defects such as data are not accurate enough, abnormal conditions are many and the load of Moisture Meter is high, it is provided that a kind of reduce cost, reduce test error in data, improve work efficiency and improve the preparation method of moisture measurement sample in Moisture Meter service life.
Therefore, first aspect, the preparation method that the invention provides a kind of moisture measurement sample, the method includes: under sampling, adds sample, and seal sample preparation bottle as test specimens in sample preparation bottle；
Or, under sampling, directly seal sample preparation bottle as blank sample；
Wherein, described sampling includes substantially invariable moisture.
Second aspect, the invention provides the detection method of a kind of moisture measurement sample, and the method includes: the preparation method described in first aspect prepares water content detection sample, and by karl Fischer potentiometric titration, the water content detection sample obtained is carried out water content detection.
The water content detection data of blank sample prepared by the present invention are accurate, it is used directly in the moisture measurement of different batches sample, without repeatedly preparing blank sample, therefore there is the advantage reducing cost, reduction test error in data, raising work efficiency and improving Moisture Meter service life.
Other features and advantages of the present invention will be described in detail in detailed description of the invention part subsequently.
Detailed description of the invention
Hereinafter the specific embodiment of the present invention is described in detail.It should be appreciated that detailed description of the invention described herein is merely to illustrate and explains the present invention, it is not limited to the present invention.
End points and any value of scope disclosed in this article are not limited to this accurate scope or value, and these scopes or value should be understood to the value comprised close to these scopes or value.For numerical range, between the endpoint value of each scope, between endpoint value and the independent point value of each scope, and between independent point value can combination with one another and obtain one or more new numerical range, these numerical rangies should be considered specifically open in this article.
Preparation method according to moisture measurement sample provided by the invention, the method includes: under sampling, adds sample, and seal sample preparation bottle as test specimens in sample preparation bottle；
Or, under sampling, directly seal sample preparation bottle as blank sample；
Wherein, described sampling includes substantially invariable moisture.
According to the present invention, it is less that substantially invariable moisture means the change of moisture in preparation process, maintains essentially in the scope not easily discovered.Moisture refers to the ratio of the moisture weight in air and air weight, and unit ppm represents.Unit " ppm " refers to millionth mass fraction, i.e. the weight of contained humidity in the air of 1,000,000 parts of weight, gross weight × 10 of the weight/air of ppm=moisture6, for instance 1ppm refers in the air of 1,000,000 kilograms containing 1 kilogram of moisture.Preferably, described substantially invariable moisture is the absolute value≤0.2ppm of moisture content fluctuation, it is preferred to the condition of≤0.1ppm (such as 0.01-0.1ppm).The method obtaining substantially invariable moisture is had no particular limits and this can be selected by those skilled in the art.Wherein, the assay method of above-mentioned moisture is moisture detector.
According to the present invention, in one preferably mode, described sampling also includes essentially constant temperature and/or inert atmosphere.
According to the present invention, it is less that essentially constant temperature means the change of temperature in preparation process, maintains essentially in the scope not easily discovered.Preferably, described essentially constant temperature is absolute value≤2 DEG C of temperature fluctuation, more preferably the condition of≤1 DEG C (such as 0.1-1 DEG C).The method obtaining essentially constant temperature is had no particular limits and this can be selected by those skilled in the art.
According to the present invention, described inert atmosphere can be provided by the noble gas of various routines.Preferably, described inert atmosphere is provided by nitrogen or argon.Wherein, described inert atmosphere refers to the oxygen content (in the oxygen quality mark) condition at below 10ppm, and unit " ppm " refers to millionth mass fraction (as previously mentioned).The method obtaining oxygen content is had no particular limits and this can be selected by those skilled in the art.Wherein, the assay method of above-mentioned oxygen content is oxygen content detector.
A preferred embodiment of the invention, described sampling includes moisture and (is more preferably below 5ppm at below 10ppm, such as 0.1-5ppm), temperature is 0-30 DEG C (being more preferably 15-25 DEG C), oxygen content (is more preferably below 5ppm at below 10ppm, such as 0.1-5ppm), wherein, in the preparation process of moisture measurement sample, absolute value≤the 0.2ppm (more preferably≤0.1ppm (such as 0.01-0.1ppm)) of moisture content fluctuation, absolute value≤2 DEG C (more preferably≤1 DEG C (such as 0.1-1 DEG C)) of temperature fluctuation.
According to the present invention, described sampling can be provided by the equipment that can keep constant humidity (preferred constant temperature and/or permanent oxygen) of the various routine in this area.Preferably, described sampling is provided by vacuum glove box.
According to the present invention, when adding sample, the addition of sample is had no particular limits, if the moisture that can record in sample.Preferably, relative to the sample preparation bottle that volume is 10mL, the addition of sample is 0.01-0.5g.It is more preferably 0.04-0.1g.The internal volume of the sample preparation bottle that volume refers to.
According to the present invention, described sample can be the various samples needing to carry out moisture measurement, it is preferable that sample is various powdered chemical.Usually, sample is particle diameter D50 powdered chemical between 0.5-50 μm.Preferably, sample particle diameter is 0.1-200 μm.D50 represents that the cumulative particle sizes percentile of a sample reaches particle diameter corresponding when 50%, and its physical significance is that particle diameter accounts for 50% more than its granule, also accounts for 50% less than its granule.
Water content detection according to the present invention, the volume of sample preparation bottle had no particular limits, as long as can be smoothed out.Preferably, the volume of sample preparation bottle is 6-10mL.
Detection method according to moisture measurement sample provided by the invention, the method includes: prepares water content detection sample according to aforesaid preparation method, and by karl Fischer potentiometric titration, the water content detection sample obtained is carried out water content detection.
According to the present invention, karl Fischer titrimetry can adopt the instrument and equipment of the various routine in this area, as long as karl Fischer constant-current titration can be smoothed out.Preferably, described karl Fischer potentiometric titration detection moisture is undertaken by cassette cooker (860 cassette cookers as logical in Switzerland 10000) and Moisture Meter (as KF831 Moisture Meter is led in Switzerland ten thousand).
Hereinafter will be described the present invention by embodiment.The battery material that the sample used in following example is the different batches that Guizhou Anda Technology Energy Co., Ltd. produces (is mainly composed of LiFePO4, particle diameter D50 is 1.6 μm, particle diameter is 0.2-10 μm), sample preparation bottle tests Science and Technology Co., Ltd. purchased from Town in Shanghai spectrum, and volume is 10mL；Vacuum glove box (model is LS800S) is purchased from Delisi Industry Co., Ltd., Chengdu；860 cassette cookers and KF831 Moisture Meter are all purchased from Tong Zhong Co., Ltd of Switzerland ten thousand；The computing formula of sample moisture is: sample moisture=(test specimens absolute water content-blank sample absolute water content)/sample introduction).
By 860 cassette cookers and KF831 Moisture Meter, the step utilizing karl Fischer potentiometric titration testing moisture content is as follows:
(1) first start shooting, 860 cassette cooker temperature are adjusted to 220 DEG C；Throughput reaches 30mL/min and with empty air-tight bottle by stable for the drift value of KF831 Moisture Meter standby at 20 μ g/min；
(2) KF831 Moisture Meter is adjusted to " blank sample " pattern；
(3) the blank sample made is added inside 860 cassette cookers, through purging of gas, the moisture of blank sample is purged to inside KF831 Moisture Meter titration cup；
(4) through the test of 5min, the water content of blank sample is obtained；
(5), after blank sample is completed, KF831 Moisture Meter is adjusted to " sample test " pattern；
(6) test specimens made is added in 860 cassette cookers, in KF831 Moisture Meter operated key, input sample total amount by " ENTER ", then press " START " and start test；
(7) through the test of 5min, Moisture Meter screen would indicate that the moisture of test specimens absolute water content, blank sample water content and sample.
Embodiment 1
In vacuum glove box, pass into nitrogen, and the environmental condition in vacuum glove box maintained moisture Control for 0.4ppm ± 0.1ppm), temperature is 20 DEG C ± 1 DEG C, and oxygen content is 3ppm.Being sealed by sample preparation bottle in vacuum glove box and prepare blank sample, it addition, add 0.0782g sample in sample preparation bottle, and sealing prepares test specimens.By 860 cassette cookers and KF831 Moisture Meter, utilizing the absolute water content that karl Fischer titrimetry records in blank sample is 2.5 μ g；Absolute water content in test specimens is 45.6 μ g；Calculating sample moisture is 551.2ppm.
In ensuing three weeks, repeat the method described in embodiment 1 once weekly, in sample preparation bottle, add quality respectively 0.0523g, 0.0674g and the 0.0791g of sample；Record absolute water content respectively 2.4 μ g, the 2.5 μ g and 2.5 μ g in blank sample respectively；Record the respectively 31.3 μ g of the absolute water content in test specimens, 39.9 μ g and 46.2 μ g respectively；Calculating sample moisture respectively is 552.6ppm, 554.9ppm and 551.2ppm.
Embodiment 2
In vacuum glove box, pass into nitrogen, and the environmental condition in vacuum glove box maintains moisture be 0.5ppm ± 0.1ppm), temperature is 20 DEG C ± 1 DEG C, and oxygen content is 1ppm.In vacuum glove box, sample preparation bottle is sealed and prepare blank sample, in sample preparation bottle, additionally add 0.0481g sample, and sealing prepares test specimens.By 860 cassette cookers and KF831 Moisture Meter, utilizing the absolute water content that karl Fischer titrimetry records in blank sample is 2.5 μ g；Absolute water content in test specimens is 50.7 μ g；Calculating sample moisture is 1002.1ppm.
In ensuing three weeks, repeat the method described in embodiment 2 once weekly, in sample preparation bottle, add quality respectively 0.0607g, 0.0413g and the 0.0523g of sample；Record absolute water content respectively 2.5 μ g, the 2.4 μ g and 2.5 μ g in blank sample respectively；Record the respectively 63.6 μ g of the absolute water content in test specimens, 43.9 μ g and 54.7 μ g respectively；Calculating sample moisture respectively is 1006.6ppm, 1004.8ppm and 998ppm.
Embodiment 3
In vacuum glove box, pass into argon, and the environmental condition maintenance moisture in vacuum glove box controlled as 2ppm ± 0.1ppm), temperature is 25 DEG C ± 2 DEG C, and oxygen content is 5ppm.In vacuum glove box, sample preparation bottle is sealed and prepare blank sample, in sample preparation bottle, additionally add 0.0602g sample, and sealing prepares test specimens.By 860 cassette cookers and KF831 Moisture Meter, utilizing the absolute water content that karl Fischer titrimetry records in blank sample is 2.6 μ g；Absolute water content in test specimens is 24.1 μ g；Calculating sample moisture is 357.1ppm.
In ensuing three weeks, repeat the method described in embodiment 3 once weekly, in sample preparation bottle, add quality respectively 0.0713g, 0.0427g and the 0.0580g of sample；Record absolute water content respectively 2.7 μ g, the 2.6 μ g and 2.6 μ g in blank sample respectively；Record the respectively 28.3 μ g of the absolute water content in test specimens, 17.8 μ g and 23.5 μ g respectively；Calculating sample moisture respectively is 359.0ppm, 356.0ppm and 360.3ppm.
Comparative example 1
Prepare according to the method for embodiment 1 and detect blank sample and test specimens, the difference is that, (moisture is 9000ppm ± 2000ppm to whole process in room conditions, temperature is 25 DEG C ± 5 DEG C, oxygen content is 21 weight %) carry out, in vacuum glove box, sample preparation bottle is sealed and prepare blank sample, in sample preparation bottle, additionally add 0.0483g sample；By 860 cassette cookers and KF831 Moisture Meter, utilizing the absolute water content that karl Fischer titrimetry records in blank sample is 10.2 μ g；Absolute water content in test specimens is 30.7 μ g；Calculating sample moisture is 424.4ppm.
In ensuing three weeks, repeat the method described in comparative example 1 once weekly, in sample preparation bottle, add quality respectively 0.0526g, 0.0617g and the 0.0429g of sample；Record absolute water content respectively 22.3 μ g, the 5.0 μ g and 27.3 μ g in blank sample respectively；Record the respectively 41.7 μ g of the absolute water content in test specimens, 33.1 μ g and 44.4 μ g respectively；Calculating sample moisture respectively is 368.8ppm, 455.4ppm and 398.6ppm.
As can be seen from the above Examples and Comparative Examples, only control the condition of sample preparation in the framework of the present definition, the testing result of sample moisture can be comparatively accurate, and the testing result poor accuracy of sample moisture obtained in comparative example, and the blank sample prepared is easy to not reach requirements (absolute water content of blank sample should less than 10 μ g).
The preferred embodiment of the present invention described in detail above; but, the present invention is not limited to the detail in above-mentioned embodiment, in the technology concept of the present invention; technical scheme can being carried out multiple simple variant, these simple variant belong to protection scope of the present invention.
It is further to note that, each concrete technical characteristic described in above-mentioned detailed description of the invention, in reconcilable situation, it is possible to be combined by any suitable mode, in order to avoid unnecessary repetition, various possible compound modes are no longer illustrated by the present invention separately.
Additionally, can also carry out combination in any between the various different embodiment of the present invention, as long as it is without prejudice to the thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. the preparation method of a moisture measurement sample, it is characterised in that the method includes: under sampling, adds sample in sample preparation bottle, and seals sample preparation bottle as test specimens；
Or, under sampling, directly seal sample preparation bottle as blank sample；
Wherein, described sampling includes substantially invariable moisture.
2. preparation method according to claim 1, wherein, described substantially invariable moisture is the absolute value≤0.2ppm of moisture content fluctuation, it is preferred to the condition of≤0.1ppm.
3. preparation method according to claim 1 and 2, wherein, described sampling also includes essentially constant temperature and/or inert atmosphere.
4. preparation method according to claim 3, wherein, described essentially constant temperature is absolute value≤2 DEG C of temperature fluctuation, it is preferred to the condition of≤1 DEG C.
5. preparation method according to claim 3, wherein, described inert atmosphere is provided by nitrogen or argon.
6. the preparation method according to claim 2 or 4, wherein, described sampling includes moisture at below 10ppm, and temperature is 0-30 DEG C, and oxygen content is at below 10ppm；Preferably, it is below 5ppm that described sampling includes moisture, and temperature is 15-25 DEG C, and oxygen content is at below 5ppm.
7. the preparation method according to any one in claim 1-6, wherein, described sampling is provided by vacuum glove box.
8. preparation method according to claim 1, wherein, when adding sample, relative to the sample preparation bottle that volume is 10mL, the addition of sample is 0.01-0.5g, it is preferred to 0.04-0.1g；Preferably, described sample is powdered chemical.
9. the detection method of a moisture measurement sample, it is characterized in that, the method includes: the preparation method described in any one in claim 1-8 prepares water content detection sample, and by karl Fischer potentiometric titration, the water content detection sample obtained is carried out water content detection.
10. detection method according to claim 9, wherein, detects moisture by karl Fischer potentiometric titration and is undertaken by cassette cooker and Moisture Meter.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110146401A (en) * | 2018-02-10 | 2019-08-20 | 天津市大桥道食品有限公司 | A kind of test method freezing water content in milk sweets |
| CN111024887A (en) * | 2019-12-11 | 2020-04-17 | 上海仪电科学仪器股份有限公司 | Moisture determination method |
| CN111912891A (en) * | 2020-09-16 | 2020-11-10 | 百杰瑞(荆门)新材料有限公司 | Moisture detection method of low-moisture lithium perchlorate |
| CN112067493A (en) * | 2020-09-16 | 2020-12-11 | 百杰瑞(荆门)新材料有限公司 | Water content detection method of anhydrous lithium iodide |
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| CN105301081A (en) * | 2015-09-14 | 2016-02-03 | 深圳市星源材质科技股份有限公司 | Method for testing moisture content of coated diaphragm of lithium ion battery |
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| CN110146401A (en) * | 2018-02-10 | 2019-08-20 | 天津市大桥道食品有限公司 | A kind of test method freezing water content in milk sweets |
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| CN111912891A (en) * | 2020-09-16 | 2020-11-10 | 百杰瑞(荆门)新材料有限公司 | Moisture detection method of low-moisture lithium perchlorate |
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