CN1016899B - Method (automic absorption) for testing ca, ba and zn contents in additive and luboil cowtaining additive - Google Patents
Method (automic absorption) for testing ca, ba and zn contents in additive and luboil cowtaining additiveInfo
- Publication number
- CN1016899B CN1016899B CN 88108152 CN88108152A CN1016899B CN 1016899 B CN1016899 B CN 1016899B CN 88108152 CN88108152 CN 88108152 CN 88108152 A CN88108152 A CN 88108152A CN 1016899 B CN1016899 B CN 1016899B
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- CN
- China
- Prior art keywords
- milliliter
- additive
- ope
- milliliters
- calcium
- 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.)
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
In the method, an additive and a test sample of lubricating oil which contains the additive are put into an acid medium, and two kinds of non-ionic surfactant and certain amount of electrolyte are used. After ultrasonic treatment, the test sample is dispersed into homogeneous oil-in-water systems to form a stable micellar structure with large diameter. The critical micelle concentration (CMC) of the stable micellar structure is 9.3*10+[-4]M lower than that of a stable micellar structure which uses negative ion-nonionic surfactant, and the surface tension is reduced to 31 dyne/ cm from 70 dyne / cm of distilled water. The emulsion of the present invention can be directly sprayed into Air-C-[2]H-[2] flame to measure the content of calcium, barium and zinc. The method of the present invention can be used for measuring the content of calcium, barium and zinc in inorganic compounds.
Description
The present invention in air-acetylene torch, measure in the adjuvant and doped lubricating oil in calcium barium zinc content, belong to calcium barium zinc Determination on content in the analytical chemistry compound, especially the mensuration for calcic barium zinc additive is particularly remarkable.
In petroleum refining industry used, the check of petrochemicals had all adopted SY2659-65, SY2658-77, three kinds of analytical approachs of SY2661-77-B to measure calcium barium zinc content in recent years.Occurred in the document afterwards adopting sample through high temperature ashing air-acetylene torch DETERMINATION OF CALCIUM BY FAAS zinc content, another kind of with laughing gas-acetylene torch aas determination barium content, sensitivity all is improved.But, laughing gas (N
2O) produce difficulty, cost an arm and a leg, do not popularize as yet and use, report now emulsion both at home and abroad and in atomic absorption spectrophotometer (AAS), measured the application of other element, but air still of no use up to now-acetylene torch atomic absorption method is measured in the adjuvant simultaneously and doped lubricating oil in calcium barium zinc analysis on Content method, ultrasonic equipment is popularized and be suitable for the stable emulsion of preparation so that use in atomic absorption spectrophotometer (AAS) in addition.
The objective of the invention is to use ultrasonic shear instrument preparation thick liquid, 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 the calcium barium zinc content in the atomic absorption spectrophotometer sample, thereby reduce the surface tension of solution, strengthen oil and the water-soluble ability of separating, improve nebulization efficiency.Mainly be to improve barium atomization temperature in air-acetylene torch in addition, 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 non-ionics together emulsification be mixed with standard emulsion, in the presence of electric matter strontium nitrate and ammonium chloride with the absorbance of air-acetylene torch bioassay standard series liquid and according to concentration drawing standard curve, measure the absorbance of sample simultaneously, calculate the content of each element in the unknown sample.
Obtain stable emulsion in order to achieve the above object, the ultrasonic technology of application of advanced on sample preparation is to OPE-1[(1-15%) department's benzene-80 dimethylbenzene-normal butyl alcohol (0.5: 1-2: 3)], OPE-2[(1-15%) Tween-80 aqueous solution], concentrated hydrochloric acid and red fuming nitric acid (RFNA) (1: 1) acid mixture, 3% 4 kind of reagent of strontium nitrate electrolyte (1-5 milli) divides the addition of different series concentration to adopt L
g(3
4) orthogonal test table determines, and found out the condition of work table-1 of ultrasonic shear instrument.Through evidence OPE-1[10% department benzene-80 dimethylbenzene-normal butyl alcohol (1: 1) solution] 1ml, OPE-2(10% Tween-80 aqueous solution) 4.5ml, acid mixture/0.2ml, the emulsion stability analysis best results that the addition of strontium nitrate 3% solution 5ml makes.It is to utilize ultrasonic energy to the cavitation of emulsified thing and form stable micellar structure, must add 10 milliliters of 4N ammonium chlorides again, gets final product etc. to be determined.
In order to obtain best analysis result reliably, this paper has investigated the element disturbing effect, evidence: the concentration ratio of calcium (Ca)/barium (Ba) is during greater than 6 times, calcium metal disturbs the mensuration of barium, wherein the ferric ion of 1.5ppm is not obvious to calcium zinc inhalation effects, aluminium, magnesium absorb 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 (seeing Table 1) effectively and accurately in solution.
SY2659-65 analytical approach system uses dissolving with hydrochloric acid with the sample ashing at present, and the calcium oxalate that makes calcium generate indissoluble precipitates from solution separates out, and filters, the precipitation sulfuric acid dissolution.With the liquor potassic permanganate titration, be about analysis time 15 hours, the SY2658-77 analytical approach is to measure the classical way of barium, sample must be after calcination becomes ashes, add dissolving with hydrochloric acid, evaporate to dryness again, the dissolving back adds sulfuric acid (1: 1) heating sedimentation again, places filtration washing, precipitation just can be finished test through high-temperature calcination, constant weight, weighing, and the processing time is also longer.The SY2661-77-B method also is with sample calcination in high temperature furnace with complexometric titration zinc content, uses the dissolving with hydrochloric acid residue then, is under 5.5 the condition, to be indicator with the xylenol orange at pH, carries out titration with the EDTA standard solution.The present invention is sophisticated equipment CSJ-III (the Kaifeng second instrument factory of ultrasonic shear instrument as preparation emulsion, this instrument only was used to shear full-bodied oil product originally), in atomic absorption spectrophotometer (AAS), use the use approach that provides new 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 reduced to 31 dynes per centimeter by distilled water 70 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, and calcium sensitivity improves about 30% than aqueous solution 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%, and more than the Ba0.05%, more than the Zn0.018%, table the-2nd below, this method recovery test, two standard oil samples all reach more than 97% through the recovery of 10 replication Ca, Ba, three kinds of elements of Zn.
For example: at first take by weighing standard 11# machine oil and each a certain amount of * of standard barium adjuvant * is 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 milliliter OPE-2 and 25 ml distilled waters; handled 5 minutes with the ultrasonic shear instrument; and transfer to * in the volumetric flask of 100 milliliters volumetric flask or 250 milliliters adds 5 milliliters more respectively in bottle strontium nitrate and 10 milliliters of 4N ammonification ammoniums of 3% with the distilled water more than 50 ℃ washing, (see Table 2 with distilled water diluting to scale working sample concentration on the atomic absorption spectrophotometer (AAS) instrument; 3).
Table 1
Voltage (V) electric current (mA) bath temperature processing time resonant frequency
110 285 50 ± 3 ℃ of 5 minutes 19.5KHz
Instrument: AA-640-13 type atomic absorption spectrophotometer (AAS) table 2
Condition: title calcium (Ca) barium (Ba) zinc (Zn)
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 5-25 5-25 1-5
Table 3
Example 1 sample example 2 samples
Standard 11# machine oil (10 mensuration) standard barium adjuvant (10 mensuration)
Elements C a Ba Zn Ba
Concentration %
Title
Standard addition % 0.40 0.80 0.20 16.75
SY2659-65% 0.40
SY2658-77% 0.80 16.75
SY2661-77-B% 0.20
Atomic absorption method % 0.41 0.78 0.20 16.35
Recovery % 102 97.30 100 97.62
Coexistence elements % Mg=0.08 S=0.46 P=0.38 S=1.01 P=0.75
Standard deviation S 0.012 0.017 0.006 0.501
Mutation COEFFICIENT K 2.86 2.5 3.03 3.1
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 the standard oil sample.
* 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 of * adding reagent in the sample preparation can not change, and shakes up successively.
* select suitable volumetric flask according to the size of constituent content in the sample.
Claims (3)
1, calcium barium zinc-content determination method in a kind of adjuvant or in the doped lubricating oil, it is characterized in that taking by weighing earlier a certain amount of 100 ml beakers of putting into of lubricating oil or adjuvant adds and to add 1 milliliter of emulsifying agent (OPE-1) successively behind 0.2 milliliter of acid mixture and emulsifying agent (OPE-2) shakes up for 4.5 milliliters, and add 25 ml distilled waters, on the ultrasonic shear instrument, handle then after 5 minutes to wash and transfer in 100 milliliters or the 250 milliliters of volumetric flasks with the distilled water more than 50 ℃, strontium nitrate and 10 milliliters of ammonium salt reagent solutions of adding 5 milliliter 3% more respectively, arrive scale, working sample concentration on the atomic absorption spectrophotometer (AAS) instrument with distilled water diluting.
2, according to the method for claim 1, its feature is that also emulsifying agent (OPE-1) proportioning is:
Department's benzene-80: [dimethylbenzene: normal butyl alcohol=1: 1]=10(gram): the 90(milliliter)
Emulsifying agent (OPE-2) proportioning is:
Tween-80: water=10(gram): the 90(milliliter)
3, according to the method for claim 1, its feature is that also the acid mixture proportioning is:
Concentrated hydrochloric acid: red fuming nitric acid (RFNA)=1: 1
Ammonium salt reagent solution concentration: 4 centinormal 1 ammonium chloride solutions.
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 CN1039655A (en) | 1990-02-14 |
| CN1016899B true 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) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2674533B1 (en) * | 1991-03-29 | 1994-08-05 | Bp Chemicals Snc | BRAKE FLUID AND METHODS OF DIFFERENTIATION AND IDENTIFICATION. |
| 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 |
-
1988
- 1988-11-23 CN CN 88108152 patent/CN1016899B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN1039655A (en) | 1990-02-14 |
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