CN107656008A - The assay method of calcium oxide content in a kind of calcium stearate - Google Patents
The assay method of calcium oxide content in a kind of calcium stearate Download PDFInfo
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- CN107656008A CN107656008A CN201710910851.3A CN201710910851A CN107656008A CN 107656008 A CN107656008 A CN 107656008A CN 201710910851 A CN201710910851 A CN 201710910851A CN 107656008 A CN107656008 A CN 107656008A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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Abstract
The invention discloses a kind of assay method of calcium oxide content in calcium stearate, its key step are as follows：Step 1：It is M to weigh quality0G calcium stearate, and it is prepared into testing sample solution；Step 2：It is C that concentration is added into the solution of step 11Mol/L disodium EDTA standard liquid (EDTA) V1Ml, untill solution clear；Step 3：Chromium black T indicator is added dropwise in the solution obtained to step 2, is then C with concentration2Mol/L magnesium chloride solution (MgCl2) volumetric soiutions are changed into bluish violet from blue-green, record the volume V of the magnesium chloride solution of consumption2ml；Then the content of calcium oxide is calculated by formula.Step of the present invention is simple, easy to operate, compared to the use that rower assay method reduces instrument, reduces cost of determination.And reduce compared to the step of rower, the deviation that the accumulation of error in operating process is brought is reduced, makes measurement result more stable.
Description
Technical field
The present invention relates to a kind of raw material chemical analysis technology field, calcium oxide content in specifically a kind of calcium stearate
Assay method.
Background technology
The white powder of calcium stearate, ethanol and ether not soluble in water, cold, it is organic to be dissolved in hot benzene, benzene and turpentine oil etc.
Solvent, it is slightly soluble in the ethanol and ether of heat.It is heated to slowly decomposing at 400 DEG C, it is flammable, meet strong acid and be decomposed into stearic acid and corresponding
Calcium salt, have hygroscopicity.Calcium stearate can make the heat stabilizer of polyvinyl chloride or the lubricant of a variety of plastic processings, releasing agent
Deng.Calcium content is measured in needing to calcium stearate after the completion of production, and traditional measuring method is surveyed using rower
Amount, the measuring principle of rower is that calcium stearate is first become calcium ion, then neutralizes wherein unnecessary acid, is tuned into strong basicity.Then
Terminal is judged with the help of calcon-carboxylic acid with EDTA standard liquids.The instrument for needing to use using the above method includes 250ml
Conical flask, electric furnace, conical hopper, filter paper, pipette and 250ml volumetric flasks.1) its key step is following to be weighed sample and (is accurate to
0.001g), it is placed in 250ml conical flasks.2) ethanol is added, nitric acid, water, conical flask is placed on electric furnace and heated slightly, is kept
Micro-boiling, untill when fatty-acid layer becomes transparent and gets together.3) normal temperature is cooled to, is filtered, and is constantly rinsed and filtered with water
Paper, litmus paper is set to stop rinsing when not showing acid to washing lotion.4) filtrate and washing lotion are moved into 250ml volumetric flasks, added water to
Scale, shake up as test solution.5) the above-mentioned test solution of pipette, extract is used, is placed in 250ml conical flasks, adds water, sodium hydroxide is added dropwise
Solution adjusts the acid-base value of test solution to pH=14, adds the calcon-carboxylic acid got ready, with disodium ethylene diamine tetraacetate standard liquid
It is terminal to be titrated to solution to be changed into pure blue from red.In terms of the mass fraction X1 of calcium oxide, numerical value is represented calcium content with %,
It is calculated as follows
In formula：
The actual concentrations of c-disodium EDTA standard liquid, mol/L；
The volume for the ethylenediamine tetra-acetic acid standard liquid that V-titration is consumed, ml；
The quality of m-sample, g；
Its value of the molal weight of M-calcium oxide is 56.08, g/mol.
Using rower method test calcium content there are problems that it is following some：
1) continuous mode is cumbersome, and step is more, and for each step if the presence of error, entirety can be caused by being continued for accumulation
Result error it is larger, be unfavorable for the control of the quality of production.
2) determining instrument that cumbersome continuous mode needs are used is more, and this also increases cost of determination.
The content of the invention
Object of the present invention is to provide a kind of step is simple, calcium oxide content in the calcium stearate of measurement deviation is reduced
Assay method, to solve the problems mentioned in the above background technology.
To achieve the above object, the present invention provides following technical scheme：
The assay method of calcium oxide content in a kind of calcium stearate, its key step are as follows：
Step 1：It is M to weigh quality0G calcium stearate, and it is prepared into testing sample solution；
Step 2：It is C that concentration is added into the solution of step 11Mol/L disodium EDTA standard liquid
(EDTA)V1Ml, untill solution clear；
Step 3：Chromium black T indicator is added dropwise in the solution obtained to step 2, is then C with concentration2Mol/L chlorination
Magnesium solution (MgCl2) volumetric soiutions are changed into bluish violet from blue-green, record the volume V of the magnesium chloride solution of consumption2ml；Then lead to
The content that formula calculates calcium oxide is crossed, calcium oxide content calculation formula is as follows：
In formula：
X1The percentage composition of-calcium oxide；
C1The actual concentrations of-EDTA standard liquids, mol/L；
C2- titration MgCl2The actual concentrations of standard liquid, mol/L；
V1- consumption titrating solution EDTA volume, ml；
V2- consumption titrating solution MgCl2Volume, ml；
M1=56.08 represent the amount of the material of calcium oxide, g/mol；
M0The quality for the calcium stearate that-expression weighs.
As the further scheme of the present invention：The preparation method of the testing sample solution is as follows：
The first step：Calcium stearate sample is weighed, is placed in conical flask；
Second step：Isopropanol is added into the conical flask of the first step, concentrated hydrochloric acid, then conical flask is placed on heater and added
Heat,
Until sample is completely dissolved；
3rd step：Ammonium cushioning liquid potassium is added into the product of second step.
As further scheme of the invention：For calcium stearate per 1g, it is necessary to add 50ml isopropanol, 1ml's is dense
The ammonium cushioning liquid potassium of hydrochloric acid and 15ml.
As further scheme of the invention：The calcium stearate mass M weighed0For 2g, the isopropanol adds
Dosage is 100ml, and the addition of the concentrated hydrochloric acid is 2ml, and the addition of the ammonium cushioning liquid potassium is 30ml.
As further scheme of the invention：The concentration C of the disodium EDTA standard liquid1=
0.1mol/L, the concentration C of described magnesium chloride solution2=0.1mol/L.
As further scheme of the invention：The conical flask uses 250ml conical flask.
As further scheme of the invention：The chromium black T indicator usage amount is 2-3 drops.
Compared with prior art, the beneficial effects of the invention are as follows：Step of the present invention is simple, easy to operate, in continuous mode
In mainly used the instruments such as conical flask, heater, pipette and acid titration bottle, reduce making for instrument compared to rower
With reducing cost of determination.And reduce compared to the step of rower, reduce the accumulation of error in operating process bring it is inclined
Difference, make measurement result more stable.
Embodiment
Technical scheme is described in more detail with reference to embodiment.
The assay method of calcium oxide content in a kind of calcium stearate, its key step are as follows：
Step 1：Testing sample solution is prepared, its main preparation methods is as follows：The first step：Weigh 2g or so stearic acid
Calcium sample (be accurate to 0.001g, its specifically the amount of weighing referring to table 1), be placed in 250ml conical flask；Second step：To first
100ml isopropanol is added in the conical flask of step, 2ml concentrated hydrochloric acid, then conical flask is placed on heater and heated, until sample
Product are completely dissolved；3rd step：30ml ammonium cushioning liquid potassium is added into the product of second step.
Step 2：V is added in the solution to be measured prepared to step 11Ml concentration is 0.1mol/L ethylenediamine tetra-acetic acid two
Sodium salt standard liquid (EDTA) makes solution clear；
Step 3：2 drop chromium black T indicators are added dropwise in the solution obtained to step 2, V is then added dropwise2Ml concentration is
0.1mol/L magnesium chloride solution (MgCl2) volumetric soiutions are changed into bluish violet from blue-green；Then calcium oxide is calculated by formula
Content, calcium oxide content calculation formula is as follows：
In formula：X1The percentage composition of-calcium oxide；
C1The actual concentrations of-EDTA standard liquids, mol/L；
C2- titration MgCl2The actual concentrations of standard liquid, mol/L；
V1- consumption titrating solution EDTA volume, ml；
V2- consumption titrating solution MgCl2Volume, ml；
M1=56.08 represent the amount of the material of calcium oxide, g/mol；
M0The quality for the calcium stearate that-expression weighs.
The step present invention determines six groups of data altogether according to the method described above, the sample size M weighed0, EDTA bodies used
Product V1And MgCl2Volume V2Refer to table 1.
Table 1 is the original data record table of calcium content in the calcium stearate measured using the inventive method
Also determine six groups of data using row calibration method simultaneously to be compared, it the results are shown in Table 2
Table 2 is the original data record table of calcium content in the calcium stearate measured using rower method
By contrast the data of Tables 1 and 2 it can be seen that the average value of six groups of data that is measured with the method for the present invention and
The six groups of data measured using rower method have identical average value, but the variance of the data measured using the inventive method
Value, which is significantly less than, using the measurement of rower method, illustrates that the method compared to the row calibration method present invention can reduce the inclined of result
Difference, measurement result are more stable.
The present invention operation principle be：Stearic acid and calcium ion are separated in organic solvent, delayed with the ammonium for adding appropriate
Solution potassium is rushed, system is tuned into meta-alkalescence, then complexing calcium ions is removed with the EDTA of excess, chlorination is used with the help of eriochrome black T
Magnesium goes to consume unnecessary EDTA, while judges terminal.
The better embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment party
Formula, can also be on the premise of present inventive concept not be departed from one skilled in the relevant art's possessed knowledge
Various changes can be made.
Claims (7)
1. the assay method of calcium oxide content in a kind of calcium stearate, it is characterised in that its key step is as follows：
Step 1：Weigh quality and be M0g calcium stearate, and be prepared into testing sample solution；
Step 2：It is C that concentration is added into the solution of step 11Mol/L disodium EDTA standard liquid (EDTA)
V1Ml, untill solution clear；
Step 3：Chromium black T indicator is added dropwise in the solution obtained to step 2, is then C with concentration2Mol/L magnesium chloride solution
(MgCl2) volumetric soiutions are changed into bluish violet from blue-green, record the volume V of the magnesium chloride solution of consumption2ml；Then formula is passed through
The content of calcium oxide is calculated, calcium oxide content calculation formula is as follows：
<mrow>
<msub>
<mi>X</mi>
<mn>1</mn>
</msub>
<mo>=</mo>
<mfrac>
<mrow>
<mo>(</mo>
<mi>C</mi>
<mn>1</mn>
<mo>&times;</mo>
<mi>V</mi>
<mn>1</mn>
<mo>-</mo>
<mi>C</mi>
<mn>2</mn>
<mo>&times;</mo>
<mi>V</mi>
<mn>2</mn>
<mo>)</mo>
</mrow>
<mrow>
<mi>M</mi>
<mn>0</mn>
<mo>&times;</mo>
<mn>1000</mn>
</mrow>
</mfrac>
<mo>&times;</mo>
<mi>M</mi>
<mn>1</mn>
<mo>&times;</mo>
<mn>100</mn>
<mi>%</mi>
</mrow>
In formula：
X1The percentage composition of-calcium oxide；
C1The actual concentrations of-EDTA standard liquids, mol/L；
C2- titration the actual concentrations of MgCl2 standard liquids, mol/L；
V1- consumption titrating solution EDTA volume, ml；
V2- consumption titrating solution MgCl2 volume, ml；
M1=56.08 represent the amount of the material of calcium oxide, g/mol；
M0The quality for the calcium stearate that-expression weighs.
2. the assay method of calcium oxide content in calcium stearate according to claim 1, it is characterised in that described to treat test sample
The preparation method of product solution is as follows：
The first step：Calcium stearate sample is weighed, is placed in conical flask；
Second step：Isopropanol is added into the conical flask of the first step, concentrated hydrochloric acid, then conical flask is placed on heater and heated,
Until sample is completely dissolved；
3rd step：Ammonium cushioning liquid potassium is added into the product of second step.
3. the assay method of calcium oxide content in calcium stearate according to claim 2, it is characterised in that the hard per 1g
Sour calcium is, it is necessary to add 50ml isopropanol, 1ml concentrated hydrochloric acid and 15ml ammonium cushioning liquid potassium.
4. the assay method of calcium oxide content in calcium stearate according to claim 2, it is characterised in that described to weigh
Calcium stearate mass M0For 2g, the addition of the isopropanol is 100ml, and the addition of the concentrated hydrochloric acid is 2ml, the ammonium
The addition of cushioning liquid potassium is 30ml.
5. the assay method of calcium oxide content in calcium stearate according to claim 1, it is characterised in that the ethylenediamine
The concentration C of Sequestrene AA standard liquid1=0.1mol/L, the concentration C of described magnesium chloride solution2=0.1mol/L.
6. the assay method of calcium oxide content in calcium stearate according to claim 1, it is characterised in that the conical flask
Using 250ml conical flask.
7. the assay method of calcium oxide content in calcium stearate according to claim 1, it is characterised in that the eriochrome black T
Indicator usage amount is 2-3 drops.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109187531A (en) * | 2018-11-14 | 2019-01-11 | 南通新邦化工科技有限公司 | The rapid detection method of barium content in the barium stearate of one specific admixture calcium carbonate |
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| CN105136785A (en) * | 2015-07-29 | 2015-12-09 | 山东西王特钢有限公司 | Metallurgical lime calcium oxide content determination method |
| CN107132222A (en) * | 2017-06-29 | 2017-09-05 | 成都光明光电股份有限公司 | The assay method of zinc oxide content in metaphosphoric acid zinc |
-
2017
- 2017-09-29 CN CN201710910851.3A patent/CN107656008A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105136785A (en) * | 2015-07-29 | 2015-12-09 | 山东西王特钢有限公司 | Metallurgical lime calcium oxide content determination method |
| CN107132222A (en) * | 2017-06-29 | 2017-09-05 | 成都光明光电股份有限公司 | The assay method of zinc oxide content in metaphosphoric acid zinc |
Non-Patent Citations (2)
| Title |
|---|
| 张殿义等: "《化妆品原料规格实用手册》", 31 December 2002 * |
| 魏良璟等: "《HG/T2424-93硬脂酸钙（轻质）》", 1 January 1994 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109187531A (en) * | 2018-11-14 | 2019-01-11 | 南通新邦化工科技有限公司 | The rapid detection method of barium content in the barium stearate of one specific admixture calcium carbonate |
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Application publication date: 20180202 |