CN1186240A - Determination of paucity water - Google Patents
Determination of paucity water Download PDFInfo
- Publication number
- CN1186240A CN1186240A CN96114156A CN96114156A CN1186240A CN 1186240 A CN1186240 A CN 1186240A CN 96114156 A CN96114156 A CN 96114156A CN 96114156 A CN96114156 A CN 96114156A CN 1186240 A CN1186240 A CN 1186240A
- Authority
- CN
- China
- Prior art keywords
- magnesium chloride
- water
- sample
- solvent
- content
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
A process for measuring micro water content in magnesium chloride includes adding molecular sieve to methanol or alcohol used to dissolving magnesium chloride, drying until the water content in solven is less 5 ppm, weighing in dry inertial gas atmosphere, and titration by Karl Fischer method. The range of measured water content is 0-5%. Its minimum can be ppm order, and the relative error is less than 10%. Its advantate is high correctness and easy operation.
Description
The present invention relates to the assay method of minor amount of water in a kind of solid matter, specifically, relate to the assay method of minor amount of water in a kind of magnesium chloride.
Magnesium chloride very easily with airborne moisture content combination, be a kind of strong water absorbent, can be as the drying agent of a lot of materials.In the magnesium chloride powder of drying, contain the water of micro-crystallization and the water of absorption.Magnesium chloride has obtained using widely in a lot of chemical industry fields, as, can be used in the catalyzer as carrier or active princlple.
In some Preparation of catalysts process, need the amount of water contained in the control magnesium chloride, therefore, just need to measure what of content of minor amount of water in the magnesium chloride.
Existing mensuration to liquid water content in the solid matter generally adopts Differential scanning calorimetry, but it is not suitable for the mensuration of carrying out minor amount of water.The method of the content of existing mensuration minor amount of water adopts classical Ka Er-Fei Xiu moisture determination method mostly, mainly is used in the mensuration of moisture content in the organic solvent.But can not directly measure the content of minor amount of water in the solid inorganic compound.
Purpose of the present invention is exactly in order to overcome the shortcoming of prior art, the Determination on content method of minor amount of water in a kind of solid magnesium chloride to be provided.
The inventor has proposed the Determination on content method of minor amount of water in a kind of solid magnesium chloride through studying for a long period of time.This method comprises the steps:
(1) solvent that will be used for dissolving magnesium chloride adds molecular sieve, carries out dried, up to solvent comprises water amount＜5ppm.
(2) in the oxygen-free atmosphere in the presence of the inert gas of drying, join in the dried solvent and dissolve fully up to sample accurately taking by weighing magnesium chloride sample to be measured, by weight percentage, the concentration of solution is 0.1～4%.
(3) get the above-mentioned solution that is dissolved with the magnesium chloride sample, add karl-Fischer reagent, with Ka Er-titration of Fei Xiu assay method to terminal.
(4) get the solvent of handling with the process (1) of the same volume of sample solution, add karl-Fischer reagent, with Ka Er-titration of Fei Xiu assay method to terminal.
(5) volume of the karl-Fischer reagent of consumption was poor during utilization (3) (4) two went on foot, and came the content of minor amount of water in the calculation sample magnesium chloride.
The solvent of above-mentioned dissolving magnesium chloride is methyl alcohol, ethanol or their potpourri.
The measurement range of the liquid water content of above-mentioned magnesium chloride is 0～5%.
Assay method of the present invention is applicable to the content of measuring water in the magnesium chloride, and method of the present invention is not subjected to the restriction of liquid water content in the magnesium chloride, is specially adapted to the mensuration of minor amount of water in the magnesium chloride.The minimum detectable activity of liquid water content can reach the ppm level, relative error in 10%, the accuracy height, easy and simple to handle.
Further describe the present invention with non-limiting instance below.Except as otherwise noted, it is pure that all reagent are analysis.
Embodiment 1
(1) preparation of karl-Fischer reagent
Reagent: iodine (three grades), absolute methanol (secondary), pyridine (secondary), sodium sulphite (three grades)
Get 84.7g iodine in the reagent bottle of a drying, add the 269ml pyridine, shake to iodine and be dissolved in fully in the pyridine, add 667ml methyl alcohol, again feeding 64g sulfur dioxide gas in this solution.This solution is karl-Fischer reagent.
(2) demarcation of karl-Fischer reagent
The karl-Fischer reagent that adds excessive preparation in the titration cell of Ka Er-Fei Xiu moisture determination instrument, drying system is 30 minutes under stirring, connect galvanometer, add the full Heshui solution 1ml of toluene (the full Heshui solution of toluene under strong agitation in 20 ℃ of constant temperature 4 hours) from injection port injection, use the karl-Fischer reagent titration immediately to terminal after injecting sample solution, the karl-Fischer reagent milliliter that record consumes is counted V.
(3) drying of solvent
Get the absolute methanol of 100ml, add the 20g molecular sieve, shake repeatedly leave standstill 10 minutes after stirring after, absolute methanol is separated with molecular sieve.Add the 20g molecular sieve again in absolute methanol, operation one is to secondary more than repeating.
(4) preparation of magnesium chloride methanol solution
Under the nitrogen protection of drying, in the stopple coupon of the good 25ml of drying, and accurately weighing (to 0.0001g) on analytical balance adds through the good absolute methanol of molecular sieve drying to scale V with the magnesium chloride sample transfer about 0.5g
3, do not stop to shake the magnesium chloride sample is dissolved in the absolute methanol fully, be made into the methanol solution of magnesium chloride.
(5) mensuration of sample
Get in the titration cell that above-mentioned methanol solution 1ml joins Ka Er-Fei Xiu moisture determination instrument, use the karl-Fischer reagent titration immediately to terminal after injecting sample solution, note the volume V of the karl-Fischer reagent of consumption
1
(6) blank test
With with the joining in the titration cell of Ka Er-Fei Xiu moisture determination instrument of the same volume of methanol solution through the good absolute methanol of molecular sieve drying, use the karl-Fischer reagent titration immediately to terminal after injecting sample solution, note the volume V of the karl-Fischer reagent of consumption
2
(7) calculate
F＝G×U×C×1000/V
H
2O(ppm)＝(V
2-V
1)×F×V
3×1000/W
Wherein:
The every ml karl-Fischer reagent of F-is equivalent to the mg number of water
The proportion of the full Heshui solution of toluene in the time of G-20 ℃, g/ml
The volume of the full Heshui solution of the toluene that U-adds, ml
The volume of the karl-Fischer reagent that V-consumes, ml
The water cut of the full Heshui solution of toluene in the time of C-20 ℃
V
1The volume of the karl-Fischer reagent of-solvent consumption, ml
V
2The volume of the karl-Fischer reagent that-sample solution consumes, ml
V
3The volume of-diluted sample, ml
The weight of W-magnesium chloride sample, g
Experimental result sees Table 1
Table 1
| Experiment | Experiment | Sample is heavy | Magnesium chloride water cut (ppm) | Relative deviation | |
| Sample | Sequence number | ???(g) | Measured value | Mean value | ????(％) |
| ???1 | ????1 | ?0.5000 | ????4180 | ????4150 | ????+0.72 |
| ????2 | ?0.5000 | ????4370 | ????+5.30 | ||
| ????3 | ?0.5000 | ????4180 | ????+0.72 | ||
| ????4 | ?0.5000 | ????3990 | ????-3.86 | ||
| ????5 | ?0.5000 | ????4370 | ????+5.30 | ||
| ????6 | ?0.5000 | ????3990 | ????-3.86 | ||
| ????7 | ?0.5000 | ????3990 | ????-3.86 | ||
| ???2 | ????1 | ?0.5000 | ????50.50 | ????50.10 | ????+0.80 |
| ????2 | ?0.5000 | ????48.48 | ????-3.23 | ||
| ????3 | ?0.5000 | ????50.50 | ????+0.80 | ||
| ????4 | ?0.5000 | ????52.52 | ????+3.23 | ||
| ????5 | ?0.5000 | ????48.48 | ????-3.23 | ||
Embodiment 2
Remove the solvent of selected sample dissolution and use ethanol instead, the example weight that takes by weighing is outside the 0.2g, and all the other are with embodiment 1.The results are shown in Table 2.
Table 2
| Experiment | Experiment | Sample is heavy | Magnesium chloride water cut (ppm) | Relative deviation | |
| Sample | Sequence number | ????(g) | Measured value | Mean value | ????(％) |
| ????1 | ????1 | ??0.2000 | ????3300 | ????0.33 | ????0.00 |
| ????2 | ??0.2000 | ????3200 | ????-3.03 | ||
| ????3 | ??0.2000 | ????3400 | ????+3.03 | ||
| ????4 | ??0.2000 | ????3500 | ????+6.06 | ||
| ????5 | ??0.2000 | ????3200 | ????-3.03 | ||
| ????6 | ??0.2000 | ????3300 | ????0.00 | ||
| ????7 | ??0.2000 | ????3400 | ????-+3.03 | ||
| ????2 | ????1 | ??0.2000 | ????63.13 | ????63.73 | ????-0.94 |
| ????2 | ??0.2000 | ????65.65 | ????+3.01 | ||
| ????3 | ??0.2000 | ????64.64 | ????+1.43 | ||
| ????4 | ??0.2000 | ????63.13 | ????-0.94 | ||
| ????5 | ??0.2000 | ????62.12 | ????-2.53 | ||
Embodiment 3
In the good methyl alcohol of drying, add a certain amount of water, measure its water cut with the method for embodiment 1, measured value and calculated value comparison the results are shown in Table 3.
Table 3
| Experiment | Methanol solution contains | The water yield (ppm) | Relative deviation |
| Sequence number | Calculated value | Measured value | ????(％) |
| ??1 | ???1232 | ????11.51 | ????+6.57 |
| ??2 | ???13.06 | ????13.42 | ????+2.76 |
| ??3 | ???15.81 | ????15.98 | ????+1.08 |
| ??4 | ???21.93 | ????21.73 | ????-0.91 |
| ??5 | ???20.04 | ????28.77 | ????+2.60 |
Claims (4)
1. the Determination on content method of minor amount of water in the magnesium chloride is characterized in that this method comprises the steps:
(1) solvent that will be used for dissolving magnesium chloride adds molecular sieve, carries out dried, up to solvent comprises water amount＜5ppm;
(2) in the oxygen-free atmosphere in the presence of the inert gas of drying, join in the dried solvent and dissolve fully up to sample with accurately taking by weighing magnesium chloride sample to be measured;
(3) get the above-mentioned solution that is dissolved with the magnesium chloride sample, add karl-Fischer reagent, with Ka Er-titration of Fei Xiu assay method to terminal;
(4) get the solvent of handling with the process (1) of the same volume of sample solution, add karl-Fischer reagent, with Ka Er-titration of Fei Xiu assay method to terminal;
(5) volume of the karl-Fischer reagent of consumption was poor during utilization (3) (4) two went on foot, and came the content of minor amount of water in the calculation sample magnesium chloride.
2. the Determination on content method of minor amount of water is characterized in that in the magnesium chloride according to claim 1, and the solvent of described dissolving magnesium chloride is methyl alcohol, ethanol or their potpourri.
3. the Determination on content method of minor amount of water is characterized in that in the magnesium chloride according to claim 1, and the measurement range of described magnesium chloride liquid water content is 0～5%.
4. the Determination on content method of minor amount of water is characterized in that in the magnesium chloride according to claim 1, and the concentration of described magnesium chloride solution is for being 0.1～4%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96114156A CN1186240A (en) | 1996-12-27 | 1996-12-27 | Determination of paucity water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96114156A CN1186240A (en) | 1996-12-27 | 1996-12-27 | Determination of paucity water |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1186240A true CN1186240A (en) | 1998-07-01 |
Family
ID=5121970
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96114156A Pending CN1186240A (en) | 1996-12-27 | 1996-12-27 | Determination of paucity water |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1186240A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100356175C (en) * | 2005-11-15 | 2007-12-19 | 上海新中化学科技有限公司 | Safety karl Fischer reagent and its preparation method |
| CN102782491A (en) * | 2010-03-01 | 2012-11-14 | 中央硝子株式会社 | Method and device for measuring water content in hydrogen fluoride-containing compound |
| CN103217352A (en) * | 2013-04-23 | 2013-07-24 | 上海绿强新材料有限公司 | Method for detecting moisture content of molecular sieve drying filter element for refrigerating system |
| CN108931606A (en) * | 2018-05-31 | 2018-12-04 | 青海盐湖工业股份有限公司 | A kind of method of pair of magnesium chloride hydrate crystallization water detection |
| CN109708990A (en) * | 2018-11-23 | 2019-05-03 | 中国电子技术标准化研究院 | The measuring method of trace moisture content in a kind of electrode material for lithium ion cell |
| CN113092663A (en) * | 2021-04-14 | 2021-07-09 | 江苏扬农化工集团有限公司 | Method for measuring moisture content in organic amine |
-
1996
- 1996-12-27 CN CN96114156A patent/CN1186240A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100356175C (en) * | 2005-11-15 | 2007-12-19 | 上海新中化学科技有限公司 | Safety karl Fischer reagent and its preparation method |
| CN102782491A (en) * | 2010-03-01 | 2012-11-14 | 中央硝子株式会社 | Method and device for measuring water content in hydrogen fluoride-containing compound |
| CN103217352A (en) * | 2013-04-23 | 2013-07-24 | 上海绿强新材料有限公司 | Method for detecting moisture content of molecular sieve drying filter element for refrigerating system |
| CN108931606A (en) * | 2018-05-31 | 2018-12-04 | 青海盐湖工业股份有限公司 | A kind of method of pair of magnesium chloride hydrate crystallization water detection |
| CN109708990A (en) * | 2018-11-23 | 2019-05-03 | 中国电子技术标准化研究院 | The measuring method of trace moisture content in a kind of electrode material for lithium ion cell |
| CN109708990B (en) * | 2018-11-23 | 2021-08-13 | 中国电子技术标准化研究院 | Method for measuring content of trace moisture in electrode material for lithium ion battery |
| CN113092663A (en) * | 2021-04-14 | 2021-07-09 | 江苏扬农化工集团有限公司 | Method for measuring moisture content in organic amine |
| CN113092663B (en) * | 2021-04-14 | 2023-06-23 | 江苏扬农化工集团有限公司 | Method for measuring moisture content in organic amine |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Wimer | Potentiometric determination of amides in acetic anhydride | |
| US8232105B1 (en) | Reagents and methods and systems using them | |
| CN110133121B (en) | Method for simultaneously measuring migration amounts of ethylenediamine, propylenediamine and hexamethylenediamine in food contact material and product | |
| CN1186240A (en) | Determination of paucity water | |
| CN108341915B (en) | Preparation method and application of horseradish peroxidase molecularly imprinted fluorescent sensing material | |
| CN1191473C (en) | Method for measuring total active sulfur in petroleum fractions | |
| CN113009048A (en) | Method for detecting content of flurarana by using dispersed solid phase extraction and liquid chromatography tandem mass spectrometry | |
| Gaur et al. | 4, 4′-Dimethyloxytrityl chloride: a reagent for the spectrophotometric determination of polymer-supported amino groups | |
| CN115343242A (en) | Method for measuring sulfamethoxazole content | |
| Rimmelin-Maury et al. | A new method for nanomolar determination of silicic acid in seawater | |
| Crompton et al. | Polarographic determination of residual acrylonitrile and styrene monomers in styrene-acrylonitrile copolymers | |
| Wu et al. | Gas chromatographic determination of nalidixic acid in tablets | |
| Vitenberg et al. | Application of gas chromatographic headspace analysis to the characterization of chemical equilibria in solutions | |
| Culp et al. | Potentiometric acid-base titrations in tetramethylurea | |
| US11733219B2 (en) | Detection reagent, detection device, and method for detecting primary amide compound | |
| Opydo et al. | Determination of Cd, Pb, Cu and Zn in wood by differential puls anodic stripping voltammetry | |
| Jabbari et al. | Protonation Constants of Valin in Different Aqueous Solutions of Dimethylsulfoxide | |
| GB2304409A (en) | Reagent for determining ene-diols, thiols and water | |
| CN114236007A (en) | Determination method of acetohydroxamic acid in wheat flour and flour treatment agent thereof | |
| SU1083111A1 (en) | Boron determination method | |
| SU1640639A1 (en) | Method of determination of mercury in solutions | |
| SU1465761A1 (en) | Method of analyzing water in dioxane | |
| CN1192235C (en) | Method for separating and analyzing hydrogen ion and ion chromatographic instrument | |
| Lanniello et al. | Square-wave voltammetric determination of acetaldehyde in povidone | |
| Mungall et al. | A Spectrophotometric Method for the Determination of Moisture and Active Hydrogen |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |