CN1039655A - The calcium barium zinc-content determination method＜atomic absorption method of adjuvant and doped lubricating oil 〉 - Google Patents
The calcium barium zinc-content determination method＜atomic absorption method of adjuvant and doped lubricating oil 〉 Download PDFInfo
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- CN1039655A CN1039655A CN 88108152 CN88108152A CN1039655A CN 1039655 A CN1039655 A CN 1039655A CN 88108152 CN88108152 CN 88108152 CN 88108152 A CN88108152 A CN 88108152A CN 1039655 A CN1039655 A CN 1039655A
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- sample
- adjuvant
- barium zinc
- ope
- calcium
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Abstract
This method is used two kinds of non-ionics and a certain amount of electrolyte with adjuvant and doped lubricating oil sample in acid medium, make sample be separated into uniform oil-in-water system through ultrasonic Treatment, to form the big stable micellar structure of diameter.It reaches 9.3 * 10 than the critical micelle concentration (CMC) of using negative ion-non-ionic surfactant is low
4M, surface tension is reduced to 31 dynes per centimeter by 70 dynes per centimeter of distilled water.
This emulsion directly sprays into Air-C
2H
2Measure calcium barium zinc content in the flame.This method also can be measured the calcium barium zinc content in the mineral compound.
Description
The present invention is at Air-C
2H
2Measure the calcium barium zinc content of adjuvant and doped lubricating oil in the flame, belong to calcium barium zinc Determination on content in the analytical chemistry compound.Especially the mensuration for calcic zinc barium adjuvant is particularly remarkable.
During this petroleum refining industry used in recent years, the check of petrochemicals had all adopted among SY2659-65, SY2658-77, the SY2661-77 three kinds of analytical approachs of method B to measure calcium barium zinc content.Occurred in the document afterwards adopting sample through high temperature ashing Air-C
2H
2Flame atomic absorption spectrometry calcium zinc content, another kind N
2O-C
2H
2Flame atomic absorption spectrometry barium content, sensitivity all is improved.But, laughing gas (N
2O) the production and supply difficulty costs an arm and a leg, and does not popularize as yet and uses.Both at home and abroad also report now emulsion and in AAS, measured the application of other element, but Air-C still of no use up to now
2H
2Flame atomic absorption method is measured calcium barium zinc analysis on Content method in adjuvant and the doped lubricating oil simultaneously.Ultrasonic equipment is not popularized and be suitable for the preparation stabilized emulsion so that use in ASS in addition.
The object of the invention is used ultrasonic shear instrument preparation emulsion, with sample in the presence of two kinds of good non-ionics of overtesting, transfer to after the shear treatment emulsification rapidly and add strontium nitrate and ammonium chloride in the volumetric flask, with calcium barium zinc content in the atomic absorption spectrophotometer sample, thereby to reduce the surface tension of solution, strengthen the dissolving power of oil and water, improve nebulization efficiency.Mainly be to improve barium in addition at Air-C
2H
2Atomization temperature in the flame is to obtain higher sensitivity.
The present invention is under the condition that does not have organic standard reagent, with standard reagent calcium carbonate, pure zinc granule, analyze the inorganic standard water solution that pure barium nitrate is made, when the PH=2 left and right sides and two kinds of nonionic phenotype surfactants together emulsification be mixed with standard emulsion, in the presence of electrolyte strontium nitrate and ammonium chloride, use Air-C
2H
2The absorbance and the drawing standard curve of flame bioassay standard series liquid are measured the absorbance of sample simultaneously, calculate the content of each element in the unknown sample
The ultrasonic technology of application of advanced on sample preparation in order to achieve the above object.OPE-1[(1-15% is adopted in test) department's benzene-80 dimethylbenzene-normal butyl alcohol (0.5: 1～2: 3)] and OPE-2[(1-15%) Tween-80 aqueous solution], think best results after 10% department benzene-80 dimethylbenzene-normal butyl alcohol (1: 1) solution O PE-1 and two kinds of compound uses of non-ionics of 10% Tween-80 aqueous solution OPE-2, adopt the acid mixture acidified sample of concentrated hydrochloric acid and red fuming nitric acid (RFNA) (1: 1), utilize the cavitation of ultrasonic energy to emulsified thing, form stable micellar structure, 3% strontium nitrate and the 5-20 milliliter 4N ammonium chloride that add 1-5ml again promptly form stable emulsion fluid.Etc. to be determined.
In order to obtain stable emulsion fluid, OPE-1, OPE-2, acid mixture and strontium nitrate electrolyte addition being adopted Lg(3 ') orthogonal test table determines, and found out the condition table-1 of ultrasonic shear instrument.Investigated the element disturbing effect, test is thought: calcium (Ca)/barium (Ba) concentration ratio is during greater than 6 times, calcium metal disturbs the mensuration of barium, and wherein the ferric ion of 1.5ppm is not obvious to calcium zinc inhalation effects, and magnalium absorbs mutually to the absorption of calcium zinc, calcium zinc does not all have influence.Simultaneously hydrochloric acid, nitric acid and the acid mixture of the two have been carried out the acidifying test.Acid mixture test effect the best.In addition, the adding of ammonium chloride can be measured the higher sample of calcium concentration effectively and accurately in solution.
Ultrasonic shear condition table-1
| Voltage (V) | Electric current (MA) | Water solution temperature | Processing time | Resonant frequency |
| 110 | 285 | 50±3℃ | 5 minutes | 19.5KHZ |
At present, the SY/2659-65 analytical approach is with the sample ashing, uses dissolving with hydrochloric acid.Make calcium generate the calcium oxalate of indissoluble, precipitation is separated out and is filtered from solution, the precipitation sulfuric acid dissolution.With the liquor potassic permanganate titration, be about analysis time 15 hours.SY2658-77 is a classical way of measuring barium, sample must add dissolving with hydrochloric acid, evaporate to dryness, dissolving back adding sulfuric acid (1: 1) heating sedimentation more again after calcination becomes ashes, place filtration washing, precipitation just can be finished test through high-temperature calcination, constant weight, weighing, and the processing time is also longer.Method B is with complexometric titration zinc content among the SY2661-77-, also is with sample calcination in high temperature furnace, uses the dissolving with hydrochloric acid residue then, is under 5.5 the condition, to be indicator with the diformazan bitter orange at PH, carries out titration with the EDTA standard solution.The present invention uses the use approach that provides new to the sophisticated equipment CSJ-III (Kaifeng second instrument factory, this instrument originally only be used to shear full-bodied oil product) of ultrasonic shear instrument as preparation emulsion in AAS for emulsion.Be characterized in that the sample preparation time short, add the use of mixed emulsifier again, reduced surface tension greatly, surface tension is that distilled water 70 dynes per centimeter are reduced to 31 dynes per centimeter, play enhanced sensitivity, solubilising, increased steady effect, improved antijamming capability and nebulization efficiency simultaneously.Standard emulsion absorbance one month stabilization time is constant.Calcium sensitivity improves about 30% than water liquid in the emulsion, and the sensitivity of barium improves 30-38%, and the sensitivity of zinc improves 15-20%.Detecting concentration range is respectively: more than the Ca0.02%, more than the Ba0.05%, more than the Zn0.018%.Show the-2nd below, this method recovery test, two standard oil samples all reach more than 97% through the recovery of three kinds of elements of 10 replication CaBaZn.
For example: at first take by weighing standard 11# machine oil and standard barium adjuvant
※Each is a certain amount of
※Be put in 100 ml beakers, add earlier 0.2 milliliter of acid mixture (red fuming nitric acid (RFNA): concentrated hydrochloric acid=1: 1) after the acidifying successively
※Add 1 milliliter of OPE-1,4.5 milliliters of OPE-2 and 25 ml distilled waters, handled 5 minutes, and wash with the distilled water more than 50 ℃ in the volumetric flask of the volumetric flask of transferring to 100 milliliters or 250 milliliters with the ultrasonic shear instrument
※, in bottle, add strontium nitrate and 10 milliliters of 4N ammonium chlorides of 5 milliliter 3% again, with distilled water diluting to scale working sample concentration on the atomic absorption spectrophotometer (AAS) instrument.
Instrument: AA-640-13 type atomic absorption spectrophotometer (AAS)
Condition: condition calcium (Ca) barium (Ba) zinc (Zn)
Wavelength A 422.6 553.6 213.8
Lamp current MA 896
Burner height mm 10 74
Slit A 3.8 9.5 3.8
Air mass flow l/min 10 10 10
Acetylene flow l/min 2.6 3.5 2.4
Expand 1 2.2 1
Combustion head angle ° 90 0 90
Curve ranges PPM 5-2 5-25 1-5
Table-2
Example 1 sample example 2 samples
Standard 11
#Machine oil (10 mensuration) standard barium adds own agent (10 mensuration)
Annotate: the standard volume of the calcium barium zinc that adds in the ※ oil sample and SY2659-65, SY2658-77, SY2661-77-B analytical approach measurement result are identical, think standard oil.
The amount of institute's calcic barium zinc must be in the range of linearity of working curve in the ※ sample sampling amount.
The order that the ※ sample preparation is added reagent can not change, and shakes up successively.
※ selects suitable volumetric flask according to the constituent content size of sample.
Claims (2)
1, the present invention is to be experimental basis with SY2659-65, SY2658-77, SY2661-77-B analytical approach.It is characterized in that having adopted on the sample preparation advanced ultrasonic technology.Department's benzene-80 dimethylbenzene-normal butyl alcohol and employing OPE-1[(1-15%) (0.5: 1-2: 3)] and Tween-80 aqueous solution OPE-2[(1-15%)] be emulsifying agent.Department's benzene-80 dimethylbenzene-normal butyl alcohol (1:1) of OPE-1[10% wherein] and the Tween-80 aqueous solution of POE-2[10%] share best results.
2, the standard emulsion of the present invention's use is can use Air-C in the presence of the electrolyte strontium nitrate
2H
2When flame mensuration addition selects addition to be 5 milliliters in 3% strontium nitrate of 1-5ml, anti-interference respond well.In addition, in solution, add in the 5-20 milliliter 4N oronain scope wherein selected amount and in the time of 10 milliliters, can measure the higher sample of calcium concentration effectively and accurately.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88108152 CN1016899B (en) | 1988-11-23 | 1988-11-23 | Method (automic absorption) for testing ca, ba and zn contents in additive and luboil cowtaining additive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88108152 CN1016899B (en) | 1988-11-23 | 1988-11-23 | Method (automic absorption) for testing ca, ba and zn contents in additive and luboil cowtaining additive |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1039655A true CN1039655A (en) | 1990-02-14 |
| CN1016899B CN1016899B (en) | 1992-06-03 |
Family
ID=4834962
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 88108152 Expired CN1016899B (en) | 1988-11-23 | 1988-11-23 | Method (automic absorption) for testing ca, ba and zn contents in additive and luboil cowtaining additive |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1016899B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0506261A1 (en) * | 1991-03-29 | 1992-09-30 | BP Chemicals Limited | Brake fluid and methods for differentiation and identification |
| CN103134791A (en) * | 2013-02-04 | 2013-06-05 | 宁波出入境检验检疫局检验检疫技术中心 | Method of applying emulsification technology to detect contents of elements in internal combustion engine oil |
-
1988
- 1988-11-23 CN CN 88108152 patent/CN1016899B/en not_active Expired
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0506261A1 (en) * | 1991-03-29 | 1992-09-30 | BP Chemicals Limited | Brake fluid and methods for differentiation and identification |
| FR2674533A1 (en) * | 1991-03-29 | 1992-10-02 | Bp Chemicals Snc | BRAKE FLUID AND METHODS OF DIFFERENTIATION AND IDENTIFICATION. |
| CN103134791A (en) * | 2013-02-04 | 2013-06-05 | 宁波出入境检验检疫局检验检疫技术中心 | Method of applying emulsification technology to detect contents of elements in internal combustion engine oil |
| CN103134791B (en) * | 2013-02-04 | 2015-08-19 | 宁波出入境检验检疫局检验检疫技术中心 | A kind of nonionic emulsifier that uses is applied to the method detecting each constituent content in I. C. engine oil |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1016899B (en) | 1992-06-03 |
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