Color indicator automatic titration instrument and application process thereof
Technical field
The present invention relates to a kind of oil acid base number pick-up unit and method, especially relate to a kind of color indicator automatic titration instrument and application process thereof for the test of oil acid base number.
Background technology
As everyone knows, present domestic and international market reaches the new highest record in history to the attention degree of oil product physical and chemical performance analysis.The pH-value test of oil product also is so, is the pH-value test that lubricating oil, hydraulic oil, engine oil all need to carry out oil product.Acid number is the index that contains acidic materials in the expression oil, and base number is the index of the oily neutral and alkali content of material of expression, both estimates one of oil product important quality index.
When measuring acid number or base number, oil product is dissolved in the toluene that contains a small amount of water and the isopropyl alcohol mixed solvent (or use other mixed solvent according to the requirement of examination criteria), make it become homogeneous system, at room temperature use respectively alkali or the sour working solution titration of standard.Indicate titration end-point by the change color of the indicator that adds or with potentiometric potential change, calculated acid number or the base number of oil product by the amount of consumption vs.The method that is used for the pH-value detection mainly contains two classes: indicator method and potentiometric titration, the inside and outside examination criteria of corresponding country mainly contains: GB/T 4945, ASTM D974 and GB/T 7304, SH/T 0251, SH/T0688, ASTM D664, ASTM D2896, ASTM D4739.Wherein, indicator method is used for the pH value of oil product, be widely used because of need not instrument and equipment, but also Shortcomings of while:
1, operating personnel's labour intensity is large, and operating efficiency is low.
2, can't airtight glass container in the titration process, the poisonous and harmful chemical reagent of volatilization can cause certain threat to experimenter healthy and safe.
3, the change color situation of color indicator can only rely on operating personnel to color feel judge, but everyone has nothing in common with each other to the vision of color, so can cause when measuring the same oil product, measurement result has larger deviation.
4, testing procedure is loaded down with trivial details, can't realize the detection scale of robotization, mass.
Summary of the invention
Purpose of the present invention is exactly to provide a kind of color indicator automatic titration instrument and application process thereof for the test of oil acid base number for the defective that overcomes above-mentioned prior art existence.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of color indicator automatic titration instrument, comprise light source, titration cell device, liquid-adding device, controller and input-output unit, described titration cell device comprises buret, test glass, stirrer and color sensor, described test glass is used for holding oil product to be detected, described buret stretches in the test glass, and connection liquid-adding device, described stirrer is located in the test glass, described light source, test glass and color sensor are positioned on the same optical axis, and described controller connects respectively liquid-adding device, controller, input-output unit and color sensor.
The pH-value that described analyser is used for oil product detects, and also is applicable to color indicator and detects as the titration of differentiating terminal point.
Described titration cell also comprises test glass base and the test glass plug of filling in test glass, and described test glass and color sensor are located on the test glass base, and described buret passes the test glass plug and extend in the test glass, and is fixed on test glass beyond the Great Wall.
Described test glass plug longitudinally offers an air hole, and test glass is provided with the O RunddichtringO beyond the Great Wall.
Described test glass is the quartz glass test glass, and the material of described test glass plug is the organic material of acid and alkali-resistance, and the material of described test glass base is engineering plastics.
Described liquid-adding device comprises silicone tube, titration fixed block, quantity tube and driven unit, described quantity tube is contained with vs, quantity tube and driven unit are located on the titration fixed block, described silicone tube connects quantity tube and buret, described driven unit connects quantity tube, promotes quantity tube and quantitatively exports vs.
Described driven unit comprises slurcam, lead screw, pushing block, drive motor and limiting plate, described lead screw is located on the titration fixed block, and be connected with drive motor, described pushing block is fixed on the lead screw, can move axially along lead screw with the rotation of lead screw, described slurcam connects quantity tube and pushing block, promotes quantity tube and quantitatively export vs under the drive of pushing block, and described limiting plate is used for limiting the shift position of pushing block.
Described input-output unit comprises keyboard, display and printer.
A kind of oil acid base number detection method of using above-mentioned color indicator automatic titration instrument may further comprise the steps:
1) oil product to be measured is packed into behind the test glass, open light source and also carry out liquid feeding by controller control liquid-adding device;
2) color sensor receives the light beam through oil product to be measured, and light signal is converted to electric signal, is sent to controller;
3) controller receives electric signal, and compares with the preset value of electric signal, if electric signal arrives setting value, then controls liquid-adding device and finishes liquid feeding;
4) obtain the consumption of vs in the liquid-adding device, and calculate the pH-value of oil product to be measured according to this consumption;
5) controller is crossed input-output unit output with the pH-value information exchange of oil product to be measured.
Described oil product to be measured adds test glass with after p-naphtholbenzine indicator, toluene and isopropyl alcohol mix.
Compared with prior art, the present invention has the following advantages:
1, the operation that the artificial volumetric soiutions dropping of implementing of reason, stirring, color are judged now all can realize by this analysis instrument, reduce operating personnel's operation intensity;
2, titration process carries out in airtight glass container, has avoided the injury of poisonous and harmful chemical reagent to experimenter's health;
3, avoid the experimenter because of the difference of colour vision, improved analysis precision;
4, this analysis instrument cooperates the sample automatic sampling apparatus, can realize that the oil acid base number is full-automatic, the testing of mass;
5, this analysis apparatus structure is simple, and volume is little, and stable performance is fit to laboratory and scene and does industry.
6, color sensor of the present invention is in testing process, and is contactless, lossless with titration reagent, do not have maintenance, guarantee and the loss of potential electrode in the potentiometric titration to replenish.
7, color sensor is applicable to shades of colour and changes, and signal stabilization can be applicable to the judgement of all colours indicator method titration end-point.
Description of drawings
Fig. 1 is structural representation of the present invention;
Fig. 2 is the structural representation of titration cell device of the present invention;
Fig. 3 is the structural representation of liquid-adding device of the present invention;
Fig. 4 is the process flow diagram of detection method of the present invention.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
Embodiment
As shown in Figure 1, a kind of color indicator automatic titration instrument, the pH-value that this analyser is used for oil product detects, and also is applicable to color indicator and detects as the titration of differentiating terminal point, has comprised light source 1, titration cell device 2, liquid-adding device 3, controller 4 and input-output unit 5.
Wherein, the concrete structure of titration cell device 2 as shown in Figure 2, buret 23, test glass 24, stirrer 25, color sensor 27, test glass base 26 and fill in the test glass plug 21 of test glass 24, test glass 24 and color sensor 27 are located on the test glass base 26, buret 23 passes test glass plug 21 and extend in the test glass 24, be fixed on the test glass plug 21, and the silicone tube 31 of connection liquid-adding device 3, test glass plug 21 longitudinally offers an air hole and is used for and the atmosphere conducting, test glass plug 21 is provided with O RunddichtringO 22, makes itself and test glass 24 contact portion sealing properties better.Test glass 24 is made by quartz glass, and good transmittance, wall thickness are even.The material of test glass plug 21 is the organic material of acid and alkali-resistance, and the material of test glass base 26 is engineering plastics.
The structure of liquid-adding device 3 as shown in Figure 3, comprise silicone tube 31, titration fixed block 32, quantity tube 33 and driven unit, be contained with vs in the quantity tube 33, quantity tube 33 and driven unit are located on the titration fixed block 32, silicone tube 31 connects quantity tube 33 and buret 23, driven unit comprises limiting plate 37, slurcam 34, lead screw 35, pushing block 36, drive motor 39 and the motor fixing plate 38 that is used for fixed drive motor 39, lead screw 35 is located on the titration fixed block 32, and be connected with drive motor 39, pushing block 36 is fixed on the lead screw 35, can move axially along lead screw 35 with the rotation of lead screw 35, slurcam 34 connects quantity tube 33 and pushing block 36, under the drive of pushing block 36, promote quantitatively output vs of quantity tube 33, the shift position of pushing block 36 is limited by two limiting plates 37, prevent that displacement is improper, guarantee the output quantity of vs.
Controller comprises control chip and the software program of correspondence and relevant peripheral circuit, generally adopts single-chip microcomputer and peripheral circuit thereof to realize, input-output unit comprises keyboard, display and printer, is used for the input instruction, output detections result etc.
A kind of oil acid base number detection method of using above-mentioned color indicator automatic titration instrument comprises step as shown in Figure 4:
1) with oil product to be measured with after p-naphtholbenzine indicator, toluene and isopropyl alcohol mix, add test glass, open light source and also carry out liquid feeding by controller control liquid-adding device;
2) color sensor receives the light beam through oil product to be measured, and light signal is converted to electric signal, is sent to controller;
3) controller receives electric signal, and compares with the preset value of electric signal, if electric signal arrives setting value, then controls liquid-adding device and finishes liquid feeding;
4) obtain the consumption of vs in the liquid-adding device, and calculate the pH-value of oil product to be measured according to this consumption;
5) controller is crossed input-output unit output with the pH-value information exchange of oil product to be measured.
Adopt this present invention according to the requirement of GB/T 4945 " petroleum products and lubricant acid number and base number determination method (color indicator method) ", acid number to oil product detects, the concentration value of the keyboard input 0.05mol/L potassium hydroxide standard solution by this analysis instrument is inputted mass value bulking value and the density value of oil product to be checked (or input) of oil product to be checked.For example, N=0.04950mol/L, W=1.772g, (or V=2ml, ρ
20=0.886g/cm
3).Then carry out the blank assay of mixed solvent, quantitatively add p-naphtholbenzine indicator, toluene and isopropyl alcohol mixed solvent in the glass test glass, 0.05mol/L potassium hydroxide standard solution is full of quantity tube, after getting rid of the bubble in the buret, buret is filled in the subassembly capping plug on the glass test glass with cup.Press start key and begin to detect, to be detected complete after, show the blank value (V of mixed solvent
0=0.01ml or TAN
0=0.02mgKOH/g), blank value is inputted analytical instrument, then oil acid value to be checked (TAN) is detected: quantitatively add p-naphtholbenzine indicator, toluene and isopropyl alcohol mixed solvent in the glass test glass, add oil product to be checked (1.772g), buret and cup are filled in the subassembly capping plug on the glass test glass.Press start key and begin to detect, to be detected complete after, show testing result (V=1.15ml, TAN=1.79mgKOH/g) or the printer output of oil product in display screen.
Wherein, oil product acid number computing formula: TAN=56.1*N* (V-V
0)/W=56.1*N* (V-V
0)/ρ
20* V
S
In the formula: the molal weight of 56.1-potassium hydroxide, g/mol;
The concentration of N-potassium hydroxide isopropyl alcohol standard solution, mol/L;
The amount of the required potassium hydroxide isopropyl alcohol of V-titration sample standard solution, ml;
V
0The amount of the blank required potassium hydroxide isopropyl alcohol standard solution of-titration, ml;
The W-sample size, g;
ρ
20-sample density, g/cm
3
V
S-volume of sample, ml.
Adopt the present invention to the requirement according to SH/T 0251 appendix A " petroleum products base number determination method (indicator method) ", the base number of oil product is detected, the concentration value of the keyboard input 0.1mol/L perchloric acid glacial acetic acid standard solution by this analysis instrument; Input mass value bulking value and the density value of oil product to be checked (or input) of oil product to be checked.(for example, N=0.9995mol/L, W=2.658g, (or V=3ml, ρ
20=0.886g/cm
3)).The blank assay of mixed solvent: quantitatively add p-naphtholbenzine indicator, sherwood oil (toluene or chlorobenzene substitute) and glacial acetic acid mixed solvent in the glass test glass.0.1mol/L perchloric acid glacial acetic acid standard solution is full of quantity tube, and behind the bubble in the eliminating buret, buret is filled in the subassembly capping plug on the glass test glass with cup.Press start key and begin to detect, to be detected complete after, show the blank value (V of mixed solvent
0=0.02ml or TBN
0=0.06mgKOH/g), blank value is inputted analytical instrument, then oil product base number to be checked (TBN) is detected: quantitatively add p-naphtholbenzine indicator, sherwood oil (toluene or chlorobenzene substitute) and glacial acetic acid mixed solvent in the glass test glass, add oil product to be checked (2.658g), buret and cup are filled in the subassembly capping plug on the glass test glass.Press start key and begin to detect, to be detected complete after, show testing result (V=3.25ml, TBN=6.76mgKOH/g) or the printer output of oil product in display screen.
Oil product base number computing formula: TBN=56.1*N* (V-V
0)/W=56.1*N* (V-V
0)/ρ
20* V
S
In the formula: the molal weight of 56.1-potassium hydroxide, g/mol;
The concentration of N-perchloric acid glacial acetic acid standard solution, mol/L;
The amount of the required perchloric acid glacial acetic acid of V-titration sample standard solution, ml;
V
0The amount of the blank required perchloric acid glacial acetic acid standard solution of-titration, ml;
The W-sample size, g;
ρ
20-sample density, g/cm
3
V
S-volume of sample, ml.