CN104181147A - Test method for determining content of sulfur in lubrication oil - Google Patents
Test method for determining content of sulfur in lubrication oil Download PDFInfo
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Abstract
The invention provides a test method for determining the content of sulfur in lubrication oil. The test method for determining the content of sulfur in the lubrication oil comprises the following steps: carrying out microwave digestion by using concentrated nitric acid to completely digest a lubrication oil sample and transforming the lubrication oil sample into an inorganic sample aqueous solution; adding an inorganic sulfur standard solution into a sulfur-free base lubrication oil microwave digestion solution according to a ratio to prepare a working standard solution; and determining the content of the sulfur in the lubrication oil under the working conditions of an inductively coupled plasma emission spectrometer ICP. According to the test method for determining the content of the sulfur in the lubrication oil, an ordinary ICP atomizer is used; a BURGENER atomizer, an oxygen introducing accessory and an import single-element organic sulfur standard sample do not need to be used; the interference of addition elements such as phosphorus, and chlorine in the lubrication oil can be avoided; the test method for determining the content of the sulfur in the lubrication oil is simple and convenient to operate, and is capable of accurately analyzing.
Description
Technical field
the present invention relates to a kind of micro-wave digestion-ICP method and measure the test method of sulfur content in lubricating oil, particularly detect the test method of sulfur content in aerooil.
Background technology
in lubricating oil, element sulphur can cause engine scuffing in lubricating oil uses, and reduces oil ageing stability, and lubricating oil is darkened, and produces special smell and thickness sediment and reduce the quality of lubricating oil, causes deterioration of lubricant.Therefore the sulfur content in lubricating oil is related to the pollution of carbonizing of engine and burn into wearing and tearing and environment.
at present, national standard method and petroleum chemical industry standard method for lubricating oil sulphur content determination are more, relate to multiple analytical instrument, as: GB/T378-90 tube oven method analytical approach, the oxidizing process of sample or the testing process of SO2 relatively waste time and energy, sulphur content determination in GB/T11140-89 petroleum products (x-ray spectrometry) analysis speed is very fast, but equipment and instrument are expensive, Wang Ailing, in " research of sulphur content determination in lubricating oil ", explanation tube oven method is measured sulphur, measurement result is subject to external environmental interference large, Measuring Time is long, be not suitable for measuring the oil product of containing metal and phosphorus additive, x-ray spectrometry measurement result is accurate, finding speed is fast, a few minutes unitary determination time, automaticity is high, measuring process is simple, but instrument and equipment expense is higher, additive element in the used lubricating oil of GB/T17476-89, in wear metal and pollutant and base oil, some element determination method (ICP) method standard can be measured sulphur, but need specific sampling device and inlet units element organic sulfur standard specimen, organic sulfur standard model has volatility simultaneously, cause that to compare measurement result by ICP method measurement result than other method on the low side, in Li Ping " improving the method for sulfur content accuracy in inductively coupled plasma atomic emission mensuration lubricating oil ", description standard goods and materials NIST SRM1622e measures, the recovery is only 87.7%.
the test method that this micro-wave digestion-ICP method is measured sulfur content in lubricating oil can be used general ICP atomizer, needn't use BURGENER atomizer, logical oxygen annex and inlet units element organic sulfur standard specimen, avoid the interference of the interpolation such as phosphorus, chlorine element in lubricating oil, analyzed accurately, easy and simple to handle.
Summary of the invention
The invention provides a kind of test method of measuring sulfur content in lubricating oil, adopt red fuming nitric acid (RFNA) micro-wave digestion, make sample catapepsis, be converted into inorganic aqueous solution; Do not add in proportion and formulate working stamndard solution in sulfur-bearing lubricating base oils micro-wave digestion liquid with inorganic sulfur standard solution; Use icp analysis instrument, select 182. 034nm element sulphur analysis spectral lines, the standard solution that is no less than 5 parts of variable concentrations is analyzed, the emissive porwer of testing standard solution, draws intensity-concentration curve; Then the lubricating oil sample to be measured through micro-wave digestion is tested, measure its emissive porwer, then calculate the sulfur content in lubricating oil sample to be measured according to above-mentioned intensity-concentration curve.This detection method can be used general ICP atomizer, needn't use BURGENER atomizer, logical oxygen annex and inlet units element organic sulfur standard specimen, has avoided the interference of the interpolation such as phosphorus, chlorine element in lubricating oil, has and analyzes accurately, feature easy and simple to handle.
The present invention can reach by following measures, comprises the steps:
(1) clear up processing: in every 0.5 g lubricating oil sample, add 10 mL red fuming nitric acid (RFNA)s, be placed in airtight heating arrangement, in 6min, be warming up to 80 DEG C from room temperature, keep 10min, then in 6min, be warming up to 120 DEG C, keep 20min, then in 6min, be warming up to 150 DEG C, keep 20min, make lubricating oil sample be converted into inorganic aqueous solution;
(2) preparing standard solution: select No. 0 lubricating base oils as base soln, by adding inorganic sulfur standard solution, after clearing up by step (1), be mixed with the standard solution that be no less than 5 kind variable concentrations of the degree of depth within the scope of 0-10PP;
(3) icp analysis method is measured sulfur content: start icp analysis instrument, select 182. 034nm element sulphur analysis spectral lines, the standard solution that is no less than 5 parts of variable concentrations is analyzed, the emissive porwer of testing standard solution, draws intensity-concentration curve; Then the lubricating oil sample to be measured through micro-wave digestion is tested, measure its emissive porwer, then calculate the sulfur content in lubricating oil sample to be measured according to above-mentioned intensity-concentration curve.
The present invention has following beneficial effect:
1) a kind of micro-wave digestion-ICP method of the present invention is measured the test method of sulfur content in lubricating oil, adopts red fuming nitric acid (RFNA) micro-wave digestion, makes sample catapepsis, is converted into inorganic samples aqueous solution; Inorganic sulfur standard solution is added in proportion in the lubricating base oils micro-wave digestion liquid of sulfur-bearing not and formulate working stamndard solution; Under inductive coupling plasma emission spectrograph ICP condition of work, measure sulfur content in lubricating oil, avoid the interference of the interpolation such as phosphorus, chlorine element in lubricating oil, can make its measurement result more quick and precisely, and stable performance, reliable and practical;
2) a kind of micro-wave digestion-ICP method of the present invention is measured the test method of sulfur content in lubricating oil, can use general ICP atomizer, needn't use BURGENER atomizer, logical oxygen annex and inlet units element organic sulfur standard specimen, analyzes accurately, easy and simple to handle;
3) a kind of micro-wave digestion-ICP method of the present invention is measured the test method of sulfur content in lubricating oil, for working sample and typical curve match, test selects not No. 0 base oil of sulfur-bearing to clear up, add corresponding inorganic sulfur mark liquid, be mixed with standard operation liquid to be measured, can eliminate the interference that matrix brings, avoid again using inlet units element organic sulfur standard specimen.
Embodiment
(1) clear up processing: accurately take 0.4 g ± 0.0100g, be accurate to 0.1mg lubricating oil sample to be measured, add 10 mL red fuming nitric acid (RFNA)s, carry out micro-wave digestion, make sample catapepsis, digestion solution is transferred in 100mL volumetric flask, wash counteracting tank and lid 3 times with water, cleansing solution is incorporated in volumetric flask, and water is settled to scale, shake up, to be measured.Micro-wave digestion condition is, power 1600W; Step 1), 80 DEG C, intensification 6min, keeps 10min; Step 2), 120 DEG C, intensification 6min, keeps 20min; Step 3), 150 DEG C, intensification 6min, keeps 20min;
(2) preparing standard solution: 100ppm inorganic sulfur standard solution is added to formulation working stamndard solution in lubricating base oils micro-wave digestion liquid (not sulfur-bearing, Conostan company of the U.S.) in proportion; Accurately take 5 0.4g ± 0.0100g, be accurate to No. 0 lubricating base oils of 0.1mg in micro-wave diminishing pot, clear up completely according to the processing of sample micro-wave digestion, 5 parts of digestion solutions after clearing up are transferred to respectively in 5 100mL volumetric flasks, in volumetric flask, add respectively 100ppm inorganic sulfur standard solution 0.00mL, 0.20 mL, 0.50mL, 1.00mL, 2.00mL, be diluted to volumetric flask scale mark with deionized water, shake up, this group liquid is working stamndard solution;
(3) icp analysis method is measured sulfur content: after lubricating oil sample micro-wave digestion to be measured changes into inorganic water sample and working stamndard solution and is ready to complete; Start plasma, after equipment is pre-thermally-stabilised, icp analysis parameters R F emissive power 1410W is set, plasma gas flow rate 12.0L/min, assisted gas flow 1.0L/min, atomization gas flow 0.85L/min, select 182. 034nm element sulphur analysis spectral lines, set up method of testing, standard solution is introduced to plasma emission spectrometer, test emissive porwer, and set up intensity-concentration curve, measure solution to be tested, measure S content in solution, calculate sulfur content by formula (1):
（1）
s weight percentage in-lubricating oil, %;
the constituent content that-software detection goes out, mg/L;
the cumulative volume of-test solution, mL, in the method
;
Independent mensuration twice, report mean value.
Embodiment mono-: the mensuration of sulfur content in 8B aerooil
(1), experiment condition determine, comprising:
A. reagent is: the reagent that sample micro-wave digestion is used adopts red fuming nitric acid (RFNA) (ρ 1.42g/mL analyzes pure), and consumption is 10 mL; Inorganic sulfur standard solution 100ppm, without No. 0 base oil (Conostan company of the U.S.) that adds element sulphur; Water is deionized water;
B. inductively coupled plasma atomic emission spectrometer (ICP) is measured the condition of work of sulfur content: comprising: 1) RF emissive power 1410W, frequency of operation 27.12MHz, plasma gas flow rate 12.0L/min, assisted gas flow 1.0L/min, atomization gas flow 0.85L/min, height of observation 0.0mm, sample introduction time delay 30s, stablize time delay 15s, single reading time 10s, reading number of times 3 times, scavenging period 10s, pump speed 30rpm, background correction mode Fitted spectrum simulation technology, element sulphur analytical wavelengths is selected S182.034nm;
C. micro-wave digestion program is as follows: power 1600W; Step 1), 6min to 80 DEG C of intensification, keeps 10min; Step 2), 6min to 120 DEG C of intensification, keeps 20min; Step 3), 6min to 150 DEG C of intensification, keeps 20min.
(2), test method, comprising:
A. the micro-wave digestion processing of sample: accurately take 0.4 g ± 0.0100g, the sample that is accurate to 0.1mg is placed in 100mL micro-wave diminishing pot, adds 10mL red fuming nitric acid (RFNA) (ρ 1.42g/mL, analyze pure), add a cover, be placed in clamping device, put into microwave dissolver and carry out micro-wave digestion; Clear up after EOP (end of program), be cooled to room temperature, solution is transferred in 100mL volumetric flask, wash counteracting tank and lid 3 times with water, cleansing solution is incorporated in volumetric flask, and water is settled to scale, shakes up, to be measured;
B. the preparation of working stamndard solution: accurately take 5 0.4g ± 0.0100g, be accurate to No. 0 lubricating base oils of 0.1mg in micro-wave diminishing pot, clear up completely according to the processing of sample micro-wave digestion, 5 parts of digestion solutions after clearing up are transferred to respectively in 5 100mL volumetric flasks, in volumetric flask, add respectively 100ppm inorganic sulfur standard solution 0.00mL, 0.20 mL, 0.50mL, 1.00mL, 2.00mL, be diluted to volumetric flask scale mark with anhydrating, shake up, this group liquid is working stamndard solution;
C. the mensuration of sample: under definite instrument condition of work, with first S0(0.0 in working curve liquid to be determined) suppressed zero, measure the luminous intensity of working curve molten sulfur element to be determined, ICP inductive coupling plasma emission spectrograph is according to sulfur content and the corresponding luminous intensity values drawing curve of measuring, the regression equation I=1842.421C+612.285 of curve, correlation coefficient r=0.99991; Measure sulfur content in lubricating oil sample with working curve with condition, calculate sulfur content by formula (1):
s weight percentage in-lubricating oil, %;
the constituent content that-software detection goes out, mg/L;
the cumulative volume of-test solution, mL, in the method
;
Independent mensuration twice, report mean value.
Sulfur content test figure in table 1 8B lubricating oil
| Sulfur content, % | No. 1 fresh oil | No. 2 fresh oils | No. 3 fresh oils | No. 1, oil after using | Use latter No. 2 |
| ≤0.14 | 0.0052% | 0.0054% | 0.013% | 0.020% | 0.018% |
(3), detection limit, the recovery determine, comprising:
A. by ready S0 working stamndard solution, measure solution element sulphur the emissive porwer of spectral line S182.034 nm 10 times by the operation steps in analyzing detecting method, its measured value is 560.915; 568.901; 556.231; 558.256; 565.789; 561.360; 550.583; 565.626; 548.987; 556.266; Computing method DL=3S/b according to JJG768-2005 about detection limit, detects and is limited to 0.0003%, meets the requirement that in lubricating oil, sulfur content detects;
B. will be ready to working stamndard, press luminous intensity and the corresponding sulfur content of the operation steps mensuration solution element sulphur in analyzing detecting method, measured value is respectively: 0.195mg/L, 0.507mg/L, 0.973mg/L, 1.499 mg/L, the recovery is respectively: 97.5%, 101.4%, 97.3%, 99.9%, meet the requirement that in lubricating oil, sulfur content detects.
(4) important parameter is determined
A. micro-wave digestion parameter is determined: ensure that lubricating oil can clear up completely, to effectively extend the serviceable life of micro-wave diminishing pot simultaneously, avoid counteracting tank to be exposed to for a long time in the environment of High Temperature High Pressure, according to analysis of experiments, sample can be destroyed to a part of C-C keys by 120 DEG C of middle high temperature, then temperature is raise, clear up unreacted sample completely, there is safety, save the energy, and the feature in serviceable life that can effectively extend counteracting tank, determine that micro-wave digestion program is as follows: power 1600W; Step 1), 6min to 80 DEG C of intensification, keeps 10min; Step 2), 6min to 120 DEG C of intensification, keeps 20min; Step 3), 6min to 150 DEG C of intensification, keeps 20min;
B. the setting of analytical parameters: the Mn of preparation 2mg/L, Pb, As standard solution, start plasma, after stable at least 15min, according to SPECTRO ARCOS operational manual, select Mn257.610nm, Pb168.216nm, Pb220.351nm, As189.042nm, operation method optimize, standard solution is introduced to plasma, adjust radio-frequency generator power, cooling gas flow, assisted gas flow, atomizer flow and height of observation, in conjunction with the excitation intensity of each spectral line, relative standard deviation (RSD) and signal-to-background ratio (BEC), the final analytical parameters of determining instrument is: power 1410 W, cold gas 12.0 L/min, secondary air 1.0 L/min, atomizer flow 0.85 L/min, height of observation 0.0mm,
C. the selection of analysis spectral line wavelength, the analysis spectral line of sulphur of recommending due to instrument is 180.731nm and 182.034nm, belongs to ultraviolet spectral line, more suitable to sulfur content in lubricating oil, by detection limit, the recovery and the accuracy of test spectral line, the analysis spectral line that 182.034nm is sulphur is selected in test;
D. for working sample and typical curve match, test selects not No. 0 base oil of sulfur-bearing to clear up, and adds corresponding inorganic sulfur mark liquid, is mixed with standard operation liquid to be measured, the interference bringing in order to eliminate matrix.
Embodiment bis-: the each method comparison of the mensuration with sulfur content in batch lubricating oil of the same race
By the comparison test of carrying out different tests method with batch aerooil of the same race, data are as follows:
Table 2 of the same race with batch in sulfur content test comparison
| Sequence number | Employing method | 1 | 2 | 3 | 4 |
| 1 | X-fluorescence | 0.0055% | 0.0052% | 0.013% | 0.018% |
| 2 | Lubricating oil direct injected ICP method | 0.0045% | 0.0053% | 0.012% | 0.020% |
| 3 | Tubular furnace burning/volumetric determination | 0.0058% | 0.0051% | 0.020% | 0.025% |
| 4 | Microwave Digestion by ICP-AES | 0.0052% | 0.0054% | 0.020% | 0.018% |
Embodiment tri-: phosphorous lubricating oil sulphur content determination comparison
Randomly draw phosphorous lubricating oil and carry out analysis of sulfur content, test figure shows that xrf analysis method, direct injected ICP method, microwave clearing ICP method test figure are consistent, but analyze data with GB/T378-90 tubular furnace and produce difference, illustrate that GB/T378-90 is not suitable for the lubricating oil that contains metal, phosphorus and chlorine additive and contain this class adjuvant, in lubricating oil, P elements affects test findings accuracy.
The comparison of the phosphorous lubricating oil sulphur content determination of table 3
Claims (1)
1. a test method of measuring sulfur content in lubricating oil, comprises the steps:
(1) clear up processing: in every 0.5 g lubricating oil sample, add 10 mL red fuming nitric acid (RFNA)s, be placed in airtight heating arrangement, in 6min, be warming up to 80 DEG C from room temperature, keep 10min, then in 6min, be warming up to 120 DEG C, keep 20min, then in 6min, be warming up to 150 DEG C, keep 20min, make lubricating oil sample be converted into inorganic aqueous solution;
(2) preparing standard solution: select No. 0 lubricating base oils as base soln, by adding inorganic sulfur standard solution, after clearing up by step (1), be mixed with the standard solution that be no less than 5 kind variable concentrations of the degree of depth within the scope of 0-10PP;
(3) icp analysis method is measured sulfur content: start icp analysis instrument, select 182. 034nm element sulphur analysis spectral lines, the standard solution that is no less than 5 parts of variable concentrations is analyzed, the emissive porwer of testing standard solution, draws intensity-concentration curve; Then the lubricating oil sample to be measured through micro-wave digestion is tested, measure its emissive porwer, then calculate the sulfur content in lubricating oil sample to be measured according to above-mentioned intensity-concentration curve.
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| CN111194404A (en) * | 2017-09-29 | 2020-05-22 | 杜邦安全与建筑公司 | Method for rapidly determining sulfur content in multiple samples |
| CN113670896A (en) * | 2021-08-25 | 2021-11-19 | 江苏省沙钢钢铁研究院有限公司 | Method for measuring sulfur content in steel rolling oily sludge |
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| CN106290804A (en) * | 2016-08-02 | 2017-01-04 | 青岛市光电工程技术研究院 | A kind of marine fuel oil sulfur content detection method, device and a kind of equipment |
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| CN108693015A (en) * | 2018-03-30 | 2018-10-23 | 张家港康得新光电材料有限公司 | A kind of PET film digestion procedure |
| CN113670896A (en) * | 2021-08-25 | 2021-11-19 | 江苏省沙钢钢铁研究院有限公司 | Method for measuring sulfur content in steel rolling oily sludge |
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Application publication date: 20141203 |