CN1114414A - Method for detecting micro soap-like matter - Google Patents
Method for detecting micro soap-like matter Download PDFInfo
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- CN1114414A CN1114414A CN 94107607 CN94107607A CN1114414A CN 1114414 A CN1114414 A CN 1114414A CN 94107607 CN94107607 CN 94107607 CN 94107607 A CN94107607 A CN 94107607A CN 1114414 A CN1114414 A CN 1114414A
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- soap
- sample
- value
- matter
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Abstract
The method for detecting trace content of soap matter with concentration at 10 to the power -5 M of magnitude order features high correctness and antiinterferance performance. Under alkaline condition, cationic surfactant solution is used for phase-splitting titration, during which spectrophotometer is used to measure light-absorbing value of organic phase for different amount of the surfactant, deriving the relationship curve between the value and the amount. extending the straight lines in opposite can obtain a value Va of crossing point on horizontal axis. A value Vb for experiment without soap is obtained in same way. The Va and Vb is substituted in formula to find out the concentration of soap matter.
Description
The present invention relates to the material concentration detection technique, specifically, relate to the micro soap-like matter content detecting method.
Soap-like matter is as the slaine of fatty acid, is present in animal tallow and the vegetable oil with the form of ester (glyceride), also can be produced by the fatty acid of gained such as oil, rosin.In fields such as chemical industry, environmental protection and field produces, all occupy critical role, can be used as water-proofing agent, lubricant, germifuge, drying agent etc.Therefore, the soap-like matter in important mensuration and the analytic product usually just is as Sodium stearate (NaC
18H
35O
2), sodium oleate (C
36H
53O
95H
2O) etc. content.Known this class measuring method mainly contains acidizing extraction method, the concentrated sulphuric acid-methyl alcohol method, perchloric acid method etc., and polarimetry (as CN92106967.7).Highly acid, the strong oxidizing property reagent that must use high concentration that these known method have not only have extremely strong corrosivity, especially human body are had harm, what have then needs through complicated separation, leaching process, equipment complexity not only, test period is also long, and directing terminal is not obvious.The method of main is present known detection soap-like matter content can only be carried out concentration and is higher than 10
-3The constant of the M order of magnitude detects, and can not provide reliable result to the detection of micro soap-like content.
The objective of the invention is to propose a kind of concentration is lower than 10
-3The soap-like matter content of M magnitude carries out accurate method for measuring.
Method of the present invention is carried out as follows: make tested sample in ealkaline buffer, under organic phase and water coexistence situation, with the soap-like matter of cationic surfactant titration aqueous phase, and detect the light absorption value of organic phase when splashing into different amount cationic surfactant at 640nm wavelength place with spectrophotometer.At any time indicate titration process with indicator and phase-splitting agent, be titration end-point when water is all transferred to organic phase when indicator shows.The cationic active agent addition (bulking value) that records and corresponding organic phase light absorption value are made the relation curve of these two amounts; Oppositely extend two straight line portioies of the curve of doing, the abscissa value of its intersection point correspondence is the cationic surfactant consumption of accurate titration, is designated as V
a
Do blank assay with same order again, promptly get the sample that does not contain soap-like matter and repeat enterprising step, try to achieve the consumption of cationic surfactant under the no soap sample situation, be designated as V
bTry to achieve the concentration of soap-like matter in the tested sample then by following formula,
N=(V
a-V
b) C is used cation activity agent concentration in the C/L formula, L is the volume of tested sample.
The used cationic active agent of this method is an analytically pure hamming (Hyamine) 1622.For making B
bValue is with respect to V
aValue difference is unlikely too big, and each measuring point all uses the hamming 1622 solution titration of close concentration.
The method of mensuration soap-like matter concentration of the present invention can be to soap-like matter concentration 10
-4M-10
-5The mensuration of M scope is effective, has solved at present 10
-3The difficult problem that the following soap-like matter content of M is difficult to accurately measure.
Adopt method of the present invention to measure micro soap-like matter content gained result's accuracy height.Its standard sample more as can be known, this law gained measuring result error is generally about 0.1%; Be no more than 0.4% at most.
Prior advantage is that the anti-interference that Yin Benfa measures micro soap-like matter content is good.Practice shows, when the organic molecule that contains in the tested sample below the 1000ppm, as alcohol, ester, carboxylic acid etc., and the following inorganic salts of 1000ppm, as sodium chloride, sodium sulphate etc. testing result there is not influence yet, its relative error of measurement still is no more than ± and 0.4%.
In addition, the execution of this method does not contact the concentrated sulphuric acid.The reagent of chemical property fiercenesses such as perchloric acid does not all have harm to human body, equipment, and helps improving environmental protection.
Below in conjunction with accompanying drawing the specific embodiment of the present invention is described in further detail, wherein:
Fig. 1 adopts the inventive method to measure micro soap-like matter content gained sample organic phase light absorption value-cationic active agent consumption relation curve;
Fig. 2 is the light absorption value-cationic active agent consumption relation curve of a kind of embodiment of the inventive method.
Embodiment 1
Getting sodium laurate (analyzing pure) that content is not less than 99% (as 99.2%), to be mixed with concentration be 5.0 * 10
-3M, 2.0 * 10
-3M, 3.0 * 10
-4M and 1.5 * 10
-5The test solution of M, standby.
Get hamming (Hyamine) 1622 (analyzing pure) and be mixed with 5.0 * 10
-3M solution is demarcated through the negative ion volumetric solution, and getting its concentration is 4.930 * 10
-3M, through dilution, obtaining concentration is 2.465 * 10 again
-3M, 4.930 * 10
-4M and 2.465 * 10
-5The cation activity solvent of M, standby.
Get 300 milliliters of the sodium carbonate liquors of 0.07M, mix for 100 milliliters, make alkaline buffer solution with the sodium bicarbonate solution of 0.07M.In above-mentioned mixed liquor, add 100 milliliters of n-propanols of crossing with naoh treatment again; Also need add 2.0 gram NaOH at last, the pH value of regulating this buffer solution is 11.
Bromophenol blue (biochemical reagents) solid is washed through twice distilled water, and the two weight ratio is 1: 50 during washing, and again through vacuum drying, and the control baking temperature is below 45 ℃; Become the indicator solution of 0.2% (W/V) then with buffer preparation.
Get 500 milliliters of branch absolute dichloromethanes, 100 milliliters of washings of sodium hydroxide solution of usefulness 2N are once left standstill after 60 minutes and are removed water, and the phase-splitting agent during as test is standby.
Pipette 5 milliliters of soap sample solution that are made into, put into graduated cylinder, move into each 10 milliliters of 0.5 milliliter of indicator that is made into and the above-mentioned buffer solution that is made into and methylene chloride again;
With the hamming 1622 solution titration of above-mentioned processing, after the blue look for the treatment of indicator performance is all transferred to organic phase from water, be titration end-point.Write down used hamming 1622 liquor capacity V
A(milliliter).
Get eight separating funnels, label is 0 respectively
#-7
#Each funnel is all put into a solution of converting with above-mentioned graduated cylinder.
To 4
#Splash into above-mentioned known VA (milliliter) hamming 1622 solution in the funnel, then splash into 3 by successively decreasing forward respectively with same intervals (as 0.1 milliliter) for the funnel of other numbering
#-1
#Funnel reaches to successively decrease backward and splashes into 5
#-7
#Soap sample test solution in hamming 1622 each funnel of amount difference titration of funnel.
To 0
#-7
#Each funnel vibrated for 20 seconds, and standing demix is 20 minutes then.Then with 0
#Organic phase in the funnel is a reference liquid, under the 640mm wavelength, measures 1 respectively
#-7
#The light absorption value of organic phase in the funnel.Make the relation curve of light absorption value (A)-hamming 1622 liquor capacity V (milliliter), as shown in Figure 1.Two straight line portioies meet at the P point among the reverse extending figure, and then P point abscissa value is the required accurate cationic active agent consumption of titration soap sample, is designated as V
a
Repeat above-mentioned steps with the sample that does not contain soap-like matter, do " blank assay ", try to achieve cationic surfactant consumption under the no soap sample situation, as the V of left figure among Fig. 1
b
With the above-mentioned V that tries to achieve
aAnd V
bValue substitution formula
N＝(V
a-V
b)C/L
C is used cation activity agent concentration in the formula, and L is the volume of tested sample.
For the accuracy of the inventive method is described.Selecting for use and analyzing pure sodium laurate is standard sample, and adopting known acidizing extraction method to record its content is 99.20%.Alternative is a standard sample with oil carboxylic acid sodium solution, and adopting known acidizing extraction titrimetry to record its concentration is 2.330 * 10
-3M, equally again with its dilution 10 times, concentration be 2.330 * 10
-4Second standard sample of M detects with four the variable concentrations sodium laurate solution and the oil carboxylic acid sodium solution of this law to preparation then, and calculates its content, obtains its relative error of standard sample separately simultaneously, and (table one) is listed in the table below
Table one
Embodiment 2
| Standard sample | Cationic titrant concentration (M) | This law detects | |
| Content or concentration | With standard sample relative error (%) | ||
| Bay 5.0 * 10 -3M acid sodium 2.0 * 10 -5M (content 3.0 * 10 -4M 99.20％)??1.5×10 -5M | ????4.93×10 -3????2.465×10 -5????4.930×10 -4????2.465×10 -5 | ?98.90％ ?99.10％ ?99.10％ ?99.07％ | ????-0.40 ????-0.10 ????-0.10 ????-0.13 |
| Oil 2.330 * 10 -3M carboxylate 2.330 * 10 -4M | ????2.465×10 -3????4.930×10 -4 | ?2.329×10 -3M ?2.330×10 -4M | ????-0.04 ????0.00 |
With precision be ten thousand/ balance weighing 0.125 gram oil hydroxy acid sodium, be mixed with 1000 milliliters of soap samples tests.Get 5 milliliters of this test solutions, add 10 milliliters of buffering agents, 10 milliliters of organic solvents, 2 indicator are 5.0 * 10 with concentration afterwards
-4Cationic active agent (hamming 1622) solution titration sample.When the difference amount of splashing into,, use spectrophotometer (53W in 640nm wavelength place
3) measure the light absorption value of organic phase.Make the relation curve of light absorption value (the A)-cationic active agent (V) that records, as shown in Figure 2, therefrom obtain V
aValue is 5.36 milliliters.Do " blank assay " with same step again, try to achieve V
bValue is 0.4 milliliter, then can try to achieve soap sample test solution concentration to be
N＝(V
a－V
b)C/L
＝(5.36－0.4)×5×10
-4/5
=4.96 * 10
-4M and then can calculate oil carboxylic acid sodium content and be
Claims (8)
1. the detection method of a micro soap-like matter is characterized in that it comprises the steps: successively
1. tested sample is placed in the ealkaline buffer;
2. with above-mentioned test solution under organic phase and water coexistence situation, use the cationic surfactant titration;
The light absorption value of organic phase when 3. detecting the above-mentioned cationic surfactant of the different amounts of titration at 640nm wavelength place with spectrophotometer;
4. indicate titration process with indicator, when indicating water all to transfer to organic phase, stop titration;
The relation curve of the organic phase of 5. drawing extinction amount and cationic active agent addition, and reverse extending two straight line portioies wherein, the abscissa value of writing down intersection point is V
a
6. repeat 1. above-mentioned-5. step with the sample that does not contain soap-like matter, the V when trying to achieve no soap sample
bValue;
7. substitution formula: N=(V
a-V
b) C/L calculates the concentration of soap-like matter in the sample, C is the concentration of used cationic active agent in the formula, L is the volume of tested sample.
2. the method for claim 1, it is characterized in that: described cationic surfactant is an analytically pure hamming (Hyamine) 1622.
3. a method as claimed in claim 1 or 2 is characterized in that described alkaline buffer is mixed by sodium carbonate liquor and sodium bicarbonate solution, also adds the n-propanol with naoh treatment, and regulating its pH value with NaOH again is 11.
4. method as claimed in claim 1 or 2, it is characterized in that: described indicator is the pure bromic acid indigo plants of biochemical reagents, is 1: 50 distilled water washed twice with it with weight ratio, and is after vacuum drying, formulated with buffering agent.
5. method as claimed in claim 1 or 2 is characterized in that: also put into the phase-splitting agent when being placed on tested sample in the ealkaline buffer, it be with analytically pure methylene chloride with the washing of 2N sodium hydroxide solution, leave standstill again and remove that water forms.
6. method as claimed in claim 3 is characterized in that: also put into the phase-splitting agent when being placed on tested sample in the ealkaline buffer, it be with analytically pure methylene chloride with the washing of 2N sodium hydroxide solution, leave standstill again and remove that water forms.
7. method as claimed in claim 4 is characterized in that: also put into the phase-splitting agent when being placed on tested sample in the ealkaline buffer, it be with analytically pure methylene chloride with the washing of 2N sodium hydroxide solution, leave standstill again and remove that water forms.
8. method as claimed in claim 7 is characterized in that: described soap sample is that 0.125 gram oil carboxylic acid sodium is made into 1000 milliliters, gets 5 milliliters in this soap sample, adds 10 milliliters of described buffering agents and indicator respectively; Used cationic active agent solution concentration is 5.0 * 10
-4
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94107607 CN1114414A (en) | 1994-07-08 | 1994-07-08 | Method for detecting micro soap-like matter |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94107607 CN1114414A (en) | 1994-07-08 | 1994-07-08 | Method for detecting micro soap-like matter |
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| Publication Number | Publication Date |
|---|---|
| CN1114414A true CN1114414A (en) | 1996-01-03 |
Family
ID=5033132
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94107607 Pending CN1114414A (en) | 1994-07-08 | 1994-07-08 | Method for detecting micro soap-like matter |
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|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1325904C (en) * | 2002-11-28 | 2007-07-11 | 华南理工大学 | Photometry of paper pulp suspension liquid colloid dissolving electric charge |
| CN106323972A (en) * | 2016-10-26 | 2017-01-11 | 桂林理工大学 | Judging device for spectrophotometric titration end point |
| CN106323971A (en) * | 2016-10-26 | 2017-01-11 | 桂林理工大学 | Method for judging titration end point by utilizing absorbancy |
-
1994
- 1994-07-08 CN CN 94107607 patent/CN1114414A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1325904C (en) * | 2002-11-28 | 2007-07-11 | 华南理工大学 | Photometry of paper pulp suspension liquid colloid dissolving electric charge |
| CN106323972A (en) * | 2016-10-26 | 2017-01-11 | 桂林理工大学 | Judging device for spectrophotometric titration end point |
| CN106323971A (en) * | 2016-10-26 | 2017-01-11 | 桂林理工大学 | Method for judging titration end point by utilizing absorbancy |
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