CN103983796A - Chemical compatibility testing method - Google Patents
Chemical compatibility testing method Download PDFInfo
- Publication number
- CN103983796A CN103983796A CN201410146594.7A CN201410146594A CN103983796A CN 103983796 A CN103983796 A CN 103983796A CN 201410146594 A CN201410146594 A CN 201410146594A CN 103983796 A CN103983796 A CN 103983796A
- Authority
- CN
- China
- Prior art keywords
- chemicals
- compatibility
- sample
- activation energy
- chemical compatibility
- 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
- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
Abstract
The invention relates to a chemical compatibility testing method, and mainly solves the problem that in the prior art chemical compatibility testing methods are complicated. According to the chemical compatibility testing method, under different heating rate conditions provided by a differential scanning calorimeter, peak value temperature and apparent activation energy corresponding to first decomposition peaks of compatibility-to-be-test chemicals and a mixture thereof are tested, and a DSC (differential scanning calorimetry) curve is drawn by use of the peak value temperature and apparent activation energy; and by computation of decomposition peak value temperature variation and apparent activation energy change fraction of a mixed system relative to a datum reference single system in the curve, compatibility of a to-be-test chemical and a contacted mater can be evaluated; by use of the technical scheme, the problem that in the prior art chemical compatibility testing methods are complicated can be well solved, and the chemical compatibility testing method can be used for chemical compatibility testing.
Description
Technical field
The present invention relates to a kind of method of testing chemicals compatibility.
Background technology
Compatibility refers to when two or more material mixes, and does not produce the ability of the segregation phenomenon of repelling each other.Be used for assessing between chemicals whether chemical reaction can occur under certain condition, and then set up in storage and transport process and prohibit and join standard.In storage and transport process, because multi-chemical stores or transports simultaneously, whether chemicals can compatiblely be mixed storage or equipped precondition, the mixed storage of mistake or equippedly will bring accident potential to accumulating.
CN201210193756.3 relates to a kind of method of measuring chemicals compatibility, it is characterized in that, comprising: the first step, the thermostatic oven of vacuum stability tester is heated to needed temperature, and constant temperature is standby, second step, by two or more chemicals samples dried to be measured, is divided into every kind of chemicals sample to be measured two parts of equivalent, respectively chooses a mixing, the 3rd step, mixed chemicals recombined sample to be measured and single chemicals sample to be measured are placed in respectively to the testing tube of described vacuum stability tester, after testing tube dress sample, subsequently silicone grease is smeared to by the ground place of described testing tube, insert in the pressure transducer of described vacuum stability tester the metal portion sealing of the pressure transducer of the ground place of described testing tube and described vacuum stability tester, the 4th step, described testing tube is connected with the vacuum pump of described vacuum stability tester, the vacuum tightness that is evacuated to described testing tube is below 0.5kPa, disconnect vacuum pump, observe pressure and change, guarantee that described testing tube good seal is air tight, if find that pressure changes obviously, again smear silicone grease, determine after described testing tube good seal, proceed in described thermostatic oven, the 5th step, by described vacuum stability tester medium-long range, control the computer program bag on computing machine, the needed time of test is set, check and start test after errorless, check and start test after errorless, in process of the test, described vacuum stability tester is transformed into digital signal by the signal of pressure transducer, by Ethernet converter netting twine, pass to remote computer, the pressure that described remote control computer records in described testing tube automatically changes, and when finishing, experiment automatically calculates according to equation for ideal gases formula the volume that described testing tube under standard state discharges gas, the 6th step, experiment finishes, and takes out testing tube and processes remaining sample, clears up described vacuum stability tester, the 7th step, relatively recombined sample and each single chemicals sample discharge the difference of gas volume.But the method complicated operation.
The present invention has solved this problem targetedly.
Summary of the invention
Technical matters to be solved by this invention is the problem of chemicals compatibility test method complicated operation in prior art, and a kind of method of new test chemicals compatibility is provided.The method, for chemicals compatibility test, has advantages of simple to operate.
For addressing the above problem, the technical solution used in the present invention is as follows: a kind of method of testing chemicals compatibility, utilize under the different heating rate conditions that compatibility chemicals to be measured and composition thereof provides at differential scanning calorimeter, test the corresponding peak temperature of the first decomposition peak and the apparent activation energy of compatibility chemicals to be measured and composition thereof, be depicted as DSC curve, by mixed system on calculated curve, with respect to the size of the change amount of the decomposition peak temperature of the independent system of positioning datum and apparent activation energy, change the size of mark, evaluate the compatibility of tested chemicals and contact material.
In technique scheme, preferably, when described recombined sample changes mark (△ E/Ea)≤20% with respect to variable quantity (△ Tmax) value≤2.0 of first decomposition peak's temperature of benchmark sample ℃ and potpourri sample with respect to the apparent activation energy of remembeing sample, tested chemicals and contact material compatibility are good.
In technique scheme, preferably, described recombined sample is with respect to variable quantity (△ Tmax) value >=5.0 of first decomposition peak's temperature of benchmark sample, and tested chemicals and contact material are incompatible.
Tested chemicals is at different temperature, because chemistry or physical change produce the variation that thermal effect can cause tested chemicals temperature.With differential scanning calorimeter, measure and record the temperature difference that changes between tested chemicals and reference substance and the relation of temperature, be depicted as DSC(Differential Scanning Calorimetry) curve, by mixed system on calculated curve with respect to the size of the change amount of the decomposition summit temperature of the independent system of positioning datum and the size of apparent activation energy change rate, evaluate the compatibility of tested chemicals and contact material, the method is simple to operate, has obtained good technique effect.
Below by embodiment, the invention will be further elaborated, but be not limited only to the present embodiment.
Embodiment
This patent adopts differential scanning calorimeter to survey the compatibility of chemicals and contact material.
[experimental technique]
Differential scanning calorimeter: temperature resolving power is 0.5 ℃;
Vacuum and inert atmosphere system: comprise that vacuum pump, gas flow take into account inert gas steel cylinder, reduction valve etc., inert gas should be nitrogen or High Purity Nitrogen, argon gas;
Crucible with cover plate: diameter is 5.0mm, height is 2.5mm, and the material of crucible is aluminium, stainless steel, nickel, aluminium oxide etc., and during test, crucible material should be compatible with sample; Sheeter etc.
1 Preparatory work of experiment
1.1 use analytical balances take respectively Alpha-alumina (doing reference substance) and each 0.0007g of tested chemicals, accurately to 0.00001g, put into respectively the crucible with cover plate, and numbering is standby.
1.2 take the tested chemicals of 0.0007g and the contact material potpourri of 1:1 in mass ratio, and exact value 0.00001g, puts into crucible, and numbering is standby; For density, differ larger sample, can change as one sees fit sampling ratio.
1.3 cover respectively cover plate by the crucible in 1.1,1.2, and on sheeter crimping; The sample that has fusion process during for intensification, should be placed on trimming sealing in aluminium matter flange crucible if desired.
2 test procedures
2.1 connect differential scanning calorimeter, preheating 20min, to through the crucible of 1.3 processing, put on the specimen holder of heating furnace of instrument, setting heating rate is 5 ℃/min, according to instrumentation step, test, test can stop when the first decomposition peak appears in DSC curve, also can when meeting the requirements of test temperature, stop, then, there is computing machine to make respectively the DSC curve of tested chemicals, contact material and potpourri.
The first decomposition peak on the DSC curve of 2.2 more tested chemicals and contact material, using its low person as benchmark the peak temperature of benchmark sample (as); The corresponding peak temperature of potpourri is compared with the peak temperature of benchmark sample, calculate recombined sample with respect to variable quantity (△ Tmax) value of first decomposition peak's temperature of benchmark sample.
If 2.3 △ Tmax are not less than 5.0 ℃, directly as test findings criterion.Judge that tested chemicals and contact material are incompatible.
If 2.4 △ Tmax are less than 5.0 ℃.Repeat 1.1 to 2.1 operation, to being decided to be the sample of benchmark and potpourri, as programming rate, be 2.5 ℃/min, 10.0 ℃/min, the DSC curve of 15.0 ℃/min respectively again, and read respectively the peak temperature of each curve.
3 result treatment
3.1 press formula (1) calculates potpourri sample with respect to the variable △ Tmax of the first decomposition peak temperature of benchmark sample;
△Tmax=Tmax1-Tmax2 （1）
In formula:
△ Tmax---potpourri sample decomposes the numerical value of the variable of peak temperature with respect to benchmark sample first, unit is ℃;
When Tmax1---programming rate is 5 ℃/min, decompose the numerical value of peak temperature as first of benchmark sample, unit is ℃;
When Tmax2---programming rate is 5 ℃/min, first of potpourri sample decomposes the numerical value of peak temperature, and unit is ℃.
3.2 use computing machine analysis process systems calculate potpourri sample and as the apparent activation energy of benchmark sample.
3.3 press formula (2) calculates potpourri sample and changes mark with respect to the apparent activation energy of benchmark sample:
△E/Ea=100×(Ea1-Ea2)/Ea1 （2）
In formula:
△ E/Ea---potpourri sample changes mark with respect to the apparent activation energy of remembeing sample, in percentage (%);
Ea1---the numerical value of benchmark sample apparent activation energy, unit is KJ/mol;
Ea2---the numerical value of potpourri sample apparent activation energy, unit is KJ/mol.
4 compatibility evaluations
The Criterion of Compatibility of tested chemicals and contact material is in Table 1:
Criterion of Compatibility between the tested chemicals of table 1 and contact material
According to table 1, for compatibility grade, be the potpourri sample of 1 grade, directly judge that tested chemicals and contact material compatibility are good; For the potpourri sample of 2 to 5 grades of compatibility grades, when using at normal temperatures and storing, should do the compatibility test of other method of testings, carried out synthetic determination.
[embodiment 1～3]
According to [experimental technique], the compatibility that adopts differential scanning calorimeter to test several chemicals.Test result is in Table 2.
Table 2
Wherein, in table 2:
2012040902: fracturing liquid rubber-breaking agent (ammonium persulfate 95%);
040912: combined polyether (polyether glycol 100%);
040935: viscosity reducer (25% AEO, 25% paregal O-20,50% water);
040937: oil-water well clean-out system (massfraction forms: 15% neopelex, 10% APES, 20% peregal o-20,55% water).
[embodiment 4～6]
According to [experimental technique], the compatibility that adopts differential scanning calorimeter to test several chemicals.Test result is in Table 3.
Table 3
Wherein, in table 2:
2011041667: microcapsule degelling agent EAB(ammonium persulfate, content >80.0% resin, content <20%);
041625: oil well cement retarder (modified starch >=90%);
041626: oil-well cement filtrate reducer (polyvinyl alcohol (PVA) >=30%, sodium sulphate >=58%, organic sulfonic acid >=8%);
041647: well cementation separant (resin >=22%, hydroxycarboxylic acid >=35%, polyacrylamide >=38%).
Claims (3)
1. a method of testing chemicals compatibility, utilize under the different heating rate conditions that compatibility chemicals to be measured and composition thereof provides at differential scanning calorimeter, test the corresponding peak temperature of the first decomposition peak and the apparent activation energy of compatibility chemicals to be measured and composition thereof, be depicted as DSC curve, by mixed system on calculated curve, with respect to the size of the change amount of the decomposition peak temperature of the independent system of positioning datum and the size of apparent activation energy variation mark, evaluate the compatibility of tested chemicals and contact material.
2. test according to claim 1 the method for chemicals compatibility, while it is characterized in that described recombined sample changes mark (△ E/Ea)≤20% with respect to variable quantity (△ Tmax) value≤2.0 of first decomposition peak's temperature of benchmark sample ℃ and potpourri sample with respect to the apparent activation energy of remembeing sample, tested chemicals and contact material compatibility are good.
3. test according to claim 1 the method for chemicals compatibility, it is characterized in that described recombined sample is with respect to variable quantity (△ Tmax) value >=5.0 of first decomposition peak's temperature of benchmark sample, tested chemicals and contact material are incompatible.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410146594.7A CN103983796A (en) | 2014-04-11 | 2014-04-11 | Chemical compatibility testing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410146594.7A CN103983796A (en) | 2014-04-11 | 2014-04-11 | Chemical compatibility testing method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103983796A true CN103983796A (en) | 2014-08-13 |
Family
ID=51275845
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410146594.7A Pending CN103983796A (en) | 2014-04-11 | 2014-04-11 | Chemical compatibility testing method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103983796A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109781571A (en) * | 2018-08-03 | 2019-05-21 | 湖北航天化学技术研究所 | A method of there are composite explosives compatibilities in the system of nitrate for evaluation |
| CN113740372A (en) * | 2020-05-28 | 2021-12-03 | 应急管理部化学品登记中心 | Method for rapidly calculating self-accelerating decomposition temperature of substance and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102680354A (en) * | 2012-06-12 | 2012-09-19 | 中国石油化工股份有限公司 | Method for determining compatibility of chemicals and application thereof |
-
2014
- 2014-04-11 CN CN201410146594.7A patent/CN103983796A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102680354A (en) * | 2012-06-12 | 2012-09-19 | 中国石油化工股份有限公司 | Method for determining compatibility of chemicals and application thereof |
Non-Patent Citations (3)
| Title |
|---|
| 岳璞等: "三种方法研究ADN与几种粘合剂的相容性", 《含能材料》, 29 February 2008 (2008-02-29), pages 66 - 69 * |
| 李思晴等: "聚乳酸与聚甲基丙烯酸甲酯相容性的研究", 《塑料工业》, 30 April 2011 (2011-04-30), pages 65 - 69 * |
| 李欢等: "用DSC研究3,3-偕二氟氨甲基氧杂环丁烷与炸药和固体推进剂组分的化学相容性", 《火炸药学报》, vol. 35, no. 4, 31 August 2012 (2012-08-31) * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109781571A (en) * | 2018-08-03 | 2019-05-21 | 湖北航天化学技术研究所 | A method of there are composite explosives compatibilities in the system of nitrate for evaluation |
| CN109781571B (en) * | 2018-08-03 | 2021-04-06 | 湖北航天化学技术研究所 | Method for evaluating compatibility of mixed explosive in system with nitrate |
| CN113740372A (en) * | 2020-05-28 | 2021-12-03 | 应急管理部化学品登记中心 | Method for rapidly calculating self-accelerating decomposition temperature of substance and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108414418B (en) | Triaxial permeability testing method | |
| CN107525720A (en) | A kind of device and method for testing compact reservoir sensitiveness | |
| CN109731531B (en) | Hydrothermal large-cavity high-temperature high-pressure experimental device and experimental method | |
| CN107727530B (en) | Application of integrated whole-course airtight gas content measuring instrument based on temperature and pressure backtracking principle | |
| CN103913279A (en) | Method and device for testing leakproofness of oil cooler by mixing helium and air | |
| CN103364241A (en) | Remodeling fine grain soil test sample preparation device | |
| CN112198093B (en) | Device and method for testing diffusion coefficient of gas in saturated live oil core | |
| CN107917868A (en) | The test device and its test method of shale suction capacity under a kind of confined pressure | |
| CN103983796A (en) | Chemical compatibility testing method | |
| CN102680354A (en) | Method for determining compatibility of chemicals and application thereof | |
| CN103760065A (en) | Test method and test system for polymer solution flow effective apparent viscosity | |
| CN101423419B (en) | Concrete impervious test piece sealant | |
| CN204903529U (en) | Major diameter rock core hollow billet pressure curve and constraint water saturation measuring device | |
| CN204903351U (en) | Three -dimensional rock specimen hole measuring device of jumbo size | |
| CN101904803B (en) | Method for preparing standard substance for detecting preservative in cosmetic | |
| CN105403657B (en) | A kind of method for testing phosphine release amount in red phosphorus flame-retardant polymeric material | |
| CN108872179B (en) | Method for measuring liquid refractive index under pressurization condition | |
| CN105403479A (en) | Determination method of bound water and free water of hardened cement paste matrix | |
| CN103116046B (en) | Preparation method for absorbing mixed fused salt carbon felt electrodes | |
| CN103969289A (en) | Method for testing compatibility of chemical through microcalorimetry | |
| CN105300865A (en) | Drilling fluid filter cake permeability testing method | |
| CN201794586U (en) | Well cementing wall packing channeling checking instrument | |
| CN103940863A (en) | Autoclave apparatus for measuring high temperature electrochemistry, and method thereof | |
| CN104280369A (en) | Method for efficiently and accurately detecting main content of industrial calcium carbonate | |
| CN106601322A (en) | VPCE static performance testing system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20140813 |