CN111579416A - Water content detection method of anhydrous lithium iodide - Google Patents
Water content detection method of anhydrous lithium iodide Download PDFInfo
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- CN111579416A CN111579416A CN202010526487.2A CN202010526487A CN111579416A CN 111579416 A CN111579416 A CN 111579416A CN 202010526487 A CN202010526487 A CN 202010526487A CN 111579416 A CN111579416 A CN 111579416A
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- lithium iodide
- anhydrous lithium
- dissolved
- anhydrous
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- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Chemical compound [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 title claims abstract description 130
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000001514 detection method Methods 0.000 title abstract description 18
- 239000000523 sample Substances 0.000 claims abstract description 85
- 239000012496 blank sample Substances 0.000 claims abstract description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 238000005070 sampling Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 4
- 239000008151 electrolyte solution Substances 0.000 description 3
- 238000011978 dissolution method Methods 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- JRMAQQQTXDJDNC-UHFFFAOYSA-M 2-ethoxy-2-oxoacetate Chemical compound CCOC(=O)C([O-])=O JRMAQQQTXDJDNC-UHFFFAOYSA-M 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/02—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content
- G01N5/025—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content for determining moisture content
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a moisture detection method of anhydrous lithium iodide, and belongs to the technical field of chemical analysis. The method for detecting the moisture of the anhydrous lithium iodide comprises the following steps: taking an anhydrous lithium iodide sample in a vacuum glove box; putting an anhydrous lithium iodide sample into a volumetric flask, and adding anhydrous ethanol to obtain a dissolved sample; putting absolute ethyl alcohol into a volumetric flask to obtain a blank sample; and taking out a part of the dissolved sample and a part of the blank sample from the vacuum glove box, and detecting on a trace moisture tester to obtain the water content of the anhydrous lithium iodide sample. The moisture detection method of anhydrous lithium iodide can obtain the moisture content of the anhydrous lithium iodide, and has the advantages of high detection precision, low cost and short detection time.
Description
Technical Field
The invention relates to the technical field of chemical analysis, in particular to a moisture detection method of anhydrous lithium iodide.
Background
With the development of new energy industry, anhydrous lithium iodide is also an important raw material applied to new energy lithium batteries, and can also be widely applied to organic synthetic chemistry.
In the prior art, the domestic anhydrous lithium iodide moisture detection adopts an electrolytic solution dissolution method, but the detection precision is low, the cost is high, and the detection time is long.
Disclosure of Invention
The invention provides a method for detecting moisture of anhydrous lithium iodide, which solves or partially solves the technical problems that in the prior art, the anhydrous lithium iodide is detected by an electrolytic solution dissolution method, but the detection precision is low, the cost is high and the detection time is long.
In order to solve the technical problem, the invention provides a moisture detection method of anhydrous lithium iodide, which comprises the following steps: taking an anhydrous lithium iodide sample in a vacuum glove box; putting an anhydrous lithium iodide sample into a volumetric flask, and adding anhydrous ethanol to obtain a dissolved sample; putting absolute ethyl alcohol into a volumetric flask to obtain a blank sample; and taking out a part of the dissolved sample and a part of the blank sample from the vacuum glove box, and detecting on a trace moisture tester to obtain the water content of the anhydrous lithium iodide sample.
Further, the taking of the anhydrous lithium iodide sample in a vacuum glove box comprises: the anhydrous lithium iodide sample was placed in a beaker.
Further, said placing the anhydrous lithium iodide sample into a volumetric flask comprises: the anhydrous lithium iodide sample in the beaker was transferred to the volumetric flask via a funnel.
Further, the taking out the partially dissolved sample and the partially blank sample from the vacuum glove box comprises: taking out at least two dissolved samples with the same volume to prepare a first parallel sample; at least two blank samples of the same volume are removed and made into a second parallel sample.
Further, the dissolved sample and the blank sample are respectively sucked through at least four disposable injection needle tubes.
Further, the obtaining the water content of the anhydrous lithium iodide sample comprises: acquiring the water mass of a dissolved sample and the water mass of a blank sample by a trace water determinator; the water content ppm of the anhydrous lithium iodide sample ═ mass of water of the dissolved sample-mass of water of the blank sample }/weight of the anhydrous lithium iodide sample.
One or more technical solutions provided in the embodiments of the present application have at least the following technical effects or advantages:
the method comprises the steps of taking an anhydrous lithium iodide sample in a vacuum glove box, putting the anhydrous lithium iodide sample into a volumetric flask, adding anhydrous ethanol to obtain a dissolved sample, putting the anhydrous ethanol into the volumetric flask to obtain a blank sample, taking a part of the dissolved sample and a part of the blank sample out of the vacuum glove box, detecting on a trace moisture detector to obtain the moisture content of the anhydrous lithium iodide sample, and obtaining the moisture content of the anhydrous lithium iodide.
Drawings
Fig. 1 is a schematic flow chart of a method for detecting moisture in anhydrous lithium iodide according to an embodiment of the present invention.
Detailed Description
Referring to fig. 1, a method for detecting moisture in anhydrous lithium iodide provided in an embodiment of the present invention includes:
step 1, taking an anhydrous lithium iodide sample in a vacuum glove box.
And 2, putting the anhydrous lithium iodide sample into a volumetric flask, and adding anhydrous ethanol to obtain a dissolved sample.
And 3, putting the absolute ethyl alcohol into a volumetric flask to obtain a blank sample.
And 4, taking out a part of the dissolved sample and a part of the blank sample from the vacuum glove box, and detecting on a trace moisture tester to obtain the water content of the anhydrous lithium iodide sample.
This application embodiment is owing to get anhydrous lithium iodide sample in vacuum glove box, put into the volumetric flask anhydrous lithium iodide sample to add anhydrous alcohol, acquire and dissolve the sample, put into the volumetric flask anhydrous alcohol, acquire blank sample, will partially dissolve sample and partial blank sample and take out vacuum glove box, and detect on the trace moisture apparatus, acquire the water content of anhydrous lithium iodide sample, can obtain the moisture content of anhydrous lithium iodide, and the detection precision is high, and is with low costs, and the check-out time is short.
Wherein, the purity of the absolute ethyl alcohol is 99.99 percent; the water content is less than 10 ppm.
The anhydrous ethanol dehydration mode is as follows: adding metal sodium and ethyl oxalate into a round-bottom flask of a reflux condenser tube, and preparing the absolute ethyl alcohol by a heating reflux mode, wherein the water content of the absolute ethyl alcohol is less than 10 ppm.
Wherein, the environmental requirements in the vacuum glove box are as follows: the relative humidity is less than or equal to 1 percent, and the accuracy of the detection result is ensured.
Step 1 is described in detail.
Taking a sample of anhydrous lithium iodide in a vacuum glove box included: the anhydrous lithium iodide sample is placed in a beaker, so that the sampling accuracy is ensured, and the mass of the sample can be accurate to 0.001 g.
Step 2 is described in detail.
Placing an anhydrous lithium iodide sample into a volumetric flask comprising: the anhydrous lithium iodide sample in the beaker is transferred into the volumetric flask through the funnel, so that the subsequent test is convenient to carry out.
Step 4 is described in detail.
Removing a portion of the dissolved sample and a portion of the blank sample from the vacuum glove box comprises:
at least two dissolved samples with the same volume are taken out to be made into a first parallel sample, and the accuracy of the experimental result is ensured.
At least two blank samples with the same volume are taken out to be made into second parallel samples, and the accuracy of the experimental result is ensured.
And respectively sucking the dissolved sample and the blank sample through at least four disposable injection needle tubes.
Obtaining the water content of the anhydrous lithium iodide sample comprises: and acquiring the water mass of the dissolved sample and the water mass of the blank sample by a trace water content tester. The water content ppm of the anhydrous lithium iodide sample ═ mass of water of the dissolved sample-mass of water of the blank sample }/weight of the anhydrous lithium iodide sample.
In order to more clearly describe the embodiments of the present invention, the following description is made in terms of the method of using the embodiments of the present invention.
Low anhydrous lithium iodide test sample 15.000g (to the nearest 0.001g) was weighed out in a 100ml beaker in order to weigh out a quantitative amount of the sample to be tested.
Transferring the weighed sample to be measured into a 100ml volumetric flask by using a funnel, adding 60ml of absolute ethyl alcohol (which releases heat when dissolved), obtaining a dissolved sample, cooling the dissolved sample to room temperature, and fixing the volume to 100ml, so as to firstly dissolve the sample to be measured and then prepare a quantitative dissolved sample.
Meanwhile, a blank sample is prepared, and electrolyte is added into a 100ml volumetric flask to reach a constant volume of 100 ml.
And shaking the prepared dissolved sample and the blank sample uniformly, respectively sucking two 2ml dissolved samples by using two disposable injection needle tubes to prepare a first parallel sample, and respectively sucking two 2ml blank samples by using two disposable injection needle tubes to prepare a second parallel sample. And taking the disposable injection needle tube out of the vacuum glove box (the treatment processes are all completed in the vacuum glove box, so that the accuracy of the result is ensured).
And detecting the first parallel sample and the second parallel sample on a trace moisture tester, recording detection data, and making a reagent blank along with the samples.
Acquiring the water mass of a dissolved sample and the water mass of a blank sample by a trace water determinator; the water content ppm of the low anhydrous lithium iodide sample is ═ water mass of the dissolved sample-water mass of the blank sample/weight of the anhydrous lithium iodide sample.
TABLE 1 electrolyte solution method vs. ethanol dissolution cost
As can be seen from table 1, the anhydrous lithium iodide sample is taken from the vacuum glove box, the anhydrous lithium iodide sample is placed in the volumetric flask, the anhydrous ethanol is added to obtain the dissolved sample, the anhydrous ethanol is placed in the volumetric flask to obtain the blank sample, the partially dissolved sample and the partially blank sample are taken out of the vacuum glove box, and the water content of the anhydrous lithium iodide sample is obtained by detecting on the trace moisture detector, so that the water content of the anhydrous lithium iodide can be obtained, the detection precision is high, the cost is low, and the detection time is short.
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to examples, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (6)
1. A method for detecting moisture in anhydrous lithium iodide is characterized by comprising the following steps:
taking an anhydrous lithium iodide sample in a vacuum glove box;
putting an anhydrous lithium iodide sample into a volumetric flask, and adding anhydrous ethanol to obtain a dissolved sample;
putting absolute ethyl alcohol into a volumetric flask to obtain a blank sample;
and taking out a part of the dissolved sample and a part of the blank sample from the vacuum glove box, and detecting on a trace moisture tester to obtain the water content of the anhydrous lithium iodide sample.
2. The method of claim 1, wherein the sampling of the anhydrous lithium iodide in a vacuum glove box comprises:
the anhydrous lithium iodide sample was placed in a beaker.
3. The method of claim 2, wherein the step of placing the sample of anhydrous lithium iodide in a volumetric flask comprises:
the anhydrous lithium iodide sample in the beaker was transferred to the volumetric flask via a funnel.
4. The method of claim 1, wherein the step of removing the partially dissolved sample and the partially blank sample from the vacuum glove box comprises:
taking out at least two dissolved samples with the same volume to prepare a first parallel sample;
at least two blank samples of the same volume are removed and made into a second parallel sample.
5. The method for detecting moisture in anhydrous lithium iodide as claimed in claim 4, wherein:
and respectively sucking the dissolved sample and the blank sample through at least four disposable injection needle tubes.
6. The method for detecting moisture content of anhydrous lithium iodide as claimed in claim 1, wherein the step of obtaining the moisture content of the anhydrous lithium iodide sample comprises:
acquiring the water mass of a dissolved sample and the water mass of a blank sample by a trace water determinator;
the water content ppm of the anhydrous lithium iodide sample ═ mass of water of the dissolved sample-mass of water of the blank sample }/weight of the anhydrous lithium iodide sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010526487.2A CN111579416A (en) | 2020-06-09 | 2020-06-09 | Water content detection method of anhydrous lithium iodide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010526487.2A CN111579416A (en) | 2020-06-09 | 2020-06-09 | Water content detection method of anhydrous lithium iodide |
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| CN111579416A true CN111579416A (en) | 2020-08-25 |
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| CN202010526487.2A Pending CN111579416A (en) | 2020-06-09 | 2020-06-09 | Water content detection method of anhydrous lithium iodide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| CN103137981A (en) * | 2013-03-06 | 2013-06-05 | 潘群生 | Preparation method for anhydrous lithium iodide |
| CN110230917A (en) * | 2019-06-17 | 2019-09-13 | 新疆骏强科技发展有限公司 | Device for drying anhydrous lithium iodide and preparation method of anhydrous lithium iodide |
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2020
- 2020-06-09 CN CN202010526487.2A patent/CN111579416A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103137981A (en) * | 2013-03-06 | 2013-06-05 | 潘群生 | Preparation method for anhydrous lithium iodide |
| CN110230917A (en) * | 2019-06-17 | 2019-09-13 | 新疆骏强科技发展有限公司 | Device for drying anhydrous lithium iodide and preparation method of anhydrous lithium iodide |
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| 安志军等: "微量水份的测定", 《计量与测试技术》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Application publication date: 20200825 |