CN116818986A - Method for measuring trace acid content in cyanoacrylate adhesive - Google Patents
Method for measuring trace acid content in cyanoacrylate adhesive Download PDFInfo
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- CN116818986A CN116818986A CN202311115849.9A CN202311115849A CN116818986A CN 116818986 A CN116818986 A CN 116818986A CN 202311115849 A CN202311115849 A CN 202311115849A CN 116818986 A CN116818986 A CN 116818986A
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- 239000002253 acid Substances 0.000 title claims abstract description 46
- 239000004830 Super Glue Substances 0.000 title claims abstract description 28
- FGBJXOREULPLGL-UHFFFAOYSA-N ethyl cyanoacrylate Chemical compound CCOC(=O)C(=C)C#N FGBJXOREULPLGL-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 14
- 238000012360 testing method Methods 0.000 claims description 245
- 239000011521 glass Substances 0.000 claims description 225
- 239000012086 standard solution Substances 0.000 claims description 122
- 239000000178 monomer Substances 0.000 claims description 113
- 229920001651 Cyanoacrylate Polymers 0.000 claims description 106
- MWCLLHOVUTZFKS-UHFFFAOYSA-N Methyl cyanoacrylate Chemical compound COC(=O)C(=C)C#N MWCLLHOVUTZFKS-UHFFFAOYSA-N 0.000 claims description 106
- 150000007530 organic bases Chemical class 0.000 claims description 103
- 239000003513 alkali Substances 0.000 claims description 101
- 238000001035 drying Methods 0.000 claims description 48
- 238000003756 stirring Methods 0.000 claims description 43
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 36
- NIQCNGHVCWTJSM-UHFFFAOYSA-N Dimethyl phthalate Chemical compound COC(=O)C1=CC=CC=C1C(=O)OC NIQCNGHVCWTJSM-UHFFFAOYSA-N 0.000 claims description 30
- 238000002156 mixing Methods 0.000 claims description 23
- ZIUSEGSNTOUIPT-UHFFFAOYSA-N ethyl 2-cyanoacetate Chemical compound CCOC(=O)CC#N ZIUSEGSNTOUIPT-UHFFFAOYSA-N 0.000 claims description 22
- ANGDWNBGPBMQHW-UHFFFAOYSA-N methyl cyanoacetate Chemical compound COC(=O)CC#N ANGDWNBGPBMQHW-UHFFFAOYSA-N 0.000 claims description 21
- FBSAITBEAPNWJG-UHFFFAOYSA-N dimethyl phthalate Natural products CC(=O)OC1=CC=CC=C1OC(C)=O FBSAITBEAPNWJG-UHFFFAOYSA-N 0.000 claims description 15
- 229960001826 dimethylphthalate Drugs 0.000 claims description 15
- 230000001112 coagulating effect Effects 0.000 claims description 12
- NQRYJNQNLNOLGT-UHFFFAOYSA-N Piperidine Chemical compound C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 claims description 8
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 6
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 3
- 238000004364 calculation method Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000007605 air drying Methods 0.000 claims 1
- 238000004458 analytical method Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000012452 mother liquor Substances 0.000 description 78
- 238000007865 diluting Methods 0.000 description 36
- 238000010586 diagram Methods 0.000 description 21
- 238000007711 solidification Methods 0.000 description 16
- 230000008023 solidification Effects 0.000 description 16
- 239000000203 mixture Substances 0.000 description 10
- 239000003381 stabilizer Substances 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 230000009969 flowable effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- IJVRPNIWWODHHA-UHFFFAOYSA-N 2-cyanoprop-2-enoic acid Chemical compound OC(=O)C(=C)C#N IJVRPNIWWODHHA-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 229930040373 Paraformaldehyde Natural products 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000861 blow drying Methods 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 229920002866 paraformaldehyde Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention belongs to the technical field of chemical analysis, and particularly relates to a method for measuring the content of trace acid in a cyanoacrylate adhesive. The invention solves the problem that the micro-acid in the cyanoacrylate adhesive is difficult to detect by adopting a titrimeter due to the too low content.
Description
Technical Field
The invention belongs to the technical field of chemical analysis, and particularly relates to a method for measuring trace acid content in cyanoacrylate adhesives.
Background
The cyanoacrylate adhesive is a type of instant adhesive taking 2-cyanoacrylate as a main component, has the advantages of high speed, strong cohesiveness and the like, and is widely used in the fields of instrument and instrument part assembly, nonferrous metal, steel, non-metal ceramic, glass, wood, flexible material rubber product adhesion and the like. The production process of the cyanoacrylate adhesive generally adopts liquid formaldehyde or paraformaldehyde and ethyl cyanoacetate as raw materials, cyclohexane is used as a dehydrating agent for production, and the cyanoacrylate adhesive mainly undergoes three stages of polymerization, depolymerization and distillation purification, and finally the refined monomer is prepared.
Sources of acidic stabilizers in the refined monomers: on one hand, trace acid contained in raw and auxiliary materials possibly enters into refined monomers along with depolymerization, distillation and purification processes; on the other hand, in order to prepare the adhesive which is convenient to store and use, other auxiliary components including acid stabilizers are added into the cyanoacrylate monomer, the acid stabilizers are usually sulfonic acid, sulfuric acid, boric acid, phosphorus pentoxide and the like, and the content of the acid stabilizers has a key influence on the storage and use of the cyanoacrylate adhesive and further adjusting and optimizing the use formula, so that the content of the acid stabilizers needs to be quantified.
The acid stabilizer content in the cyanoacrylate adhesive products currently on the market varies from a few ppm to hundreds of ppm. For products with higher acid stabilizer concentration, the content of the acid stabilizer can be detected by titration by preparing a standard titration solution by means of a titrator, but for products with lower acid stabilizer content, such as cyanoacrylate adhesive products with 3ppm-20ppm acid stabilizer content, the concentration is too low and limited by the detection limit of the titrator, so that the true value of the cyanoacrylate adhesive is difficult to obtain accurately.
Disclosure of Invention
The invention aims to provide a method for measuring the content of trace acid in cyanoacrylate adhesives, which aims to solve the problem that the accurate value cannot be obtained when the content of the acid is low in the background art.
In order to achieve the technical purpose, the technical scheme of the invention comprises the following steps:
a method for measuring the content of trace acid in cyanoacrylate adhesives comprises the following steps:
s1: taking three organic alkali standard solutions a1, a2 and a3 with sequentially increasing concentrations, wherein the concentration differences between a2 and a1 and between a3 and a2 are 30ppm,25ppm is less than a1 and less than 30ppm, and the organic alkali standard solutions are prepared by dissolving organic alkali in a neutral organic solvent;
s2: the method comprises the steps of taking three glass test tubes, placing the three glass test tubes in a constant-temperature blast drying oven for preheating for 10min, taking out the three glass test tubes, respectively weighing cyanoacrylate monomers with the same quantity, placing the cyanoacrylate monomers into the three glass test tubes, respectively adding organic alkali standard solutions with the same quantity and the same concentration of a1, a2 and a3 into the three glass test tubes, stirring and mixing the three glass test tubes, placing the three glass test tubes into the constant-temperature blast drying oven again for 15min after the three glass test tubes are uniformly mixed, and taking out the three glass test tubes for first observation after 15 min;
s3: in the first observation, if one or two cyanoacrylate monomers in three glass test tubes have fluidity, the cyanoacrylate monomers in the rest glass test tubes are in a solidification state, and then three organic alkali standard solutions b1, b2 and b3 with sequentially increasing concentrations are taken, wherein the concentration difference between b2 and b1 and between b3 and b2 is 10ppm, the concentration of b1 is greater than the greater concentration in the organic alkali standard solution for enabling the cyanoacrylate monomers to flow, and the concentration of b3 is less than the smaller concentration in the organic alkali standard solution for enabling the cyanoacrylate monomers to solidify; repeating the operation step S2, and carrying out second observation to calculate the acid content at a smaller concentration in the organic base standard solution for solidifying the cyanoacrylate monomer, wherein the calculation formula is as follows:
X=m*A/M
wherein A is the concentration of an organic base standard solution for solidifying the cyanoacrylate monomer;
the content of acid in the X-cyanoacrylate adhesive monomer;
the mass of the m-organic alkali standard solution;
the mass of the M-cyanoacrylate adhesive monomer;
in the first observation, if all cyanoacrylate monomers in the three glass test tubes have fluidity, re-taking three organic alkali standard solutions c1, c2 and c3 with sequentially increasing concentrations, wherein the concentration of c1 is greater than that of a3, the concentration differences between c1 and a3, between c2 and c1 and between c3 and c2 are 40ppm, repeating the operation step S2, and performing the third observation;
in the third observation, if one or two of the three glass test tubes have fluidity, the cyanoacrylate monomer in the remaining glass test tubes is in a coagulated state, then taking three organic base standard solutions d1, d2 and d3 with sequentially increasing concentrations, wherein the concentration difference between d2 and d1 and between d3 and d2 is 10ppm, the concentration of d1 is larger than the larger concentration in the organic base standard solution for coagulating the cyanoacrylate monomer, the concentration of d3 is smaller than the smaller concentration in the organic base standard solution for coagulating the cyanoacrylate monomer, the difference between d1 and the larger concentration in the organic base standard solution for coagulating the cyanoacrylate monomer is 10ppm, repeating the operation step S2, and performing the fourth observation to calculate the acid content from the lower concentration in the organic base standard solution for coagulating the cyanoacrylate monomer;
in the third observation, if all the cyanoacrylate monomers in the three glass test tubes are coagulated, the three organic alkali standard solutions e1, e2 and e3 with sequentially increasing concentrations are re-taken, the concentration of e1 is larger than that of a3, the concentration of e3 is smaller than that of c1, the concentration differences between e1 and a3, between e2 and e1 and between e3 and e2 are 10ppm, and the operation step S2 is repeated, wherein in the fifth observation, one or two cyanoacrylate monomers in the glass test tubes have flowability, the cyanoacrylate monomers in the rest glass test tubes are in a coagulated state, the acid content is calculated according to the lower concentration in the organic alkali standard solution for coagulating the cyanoacrylate monomers, if all the cyanoacrylate monomers in the three glass test tubes are in a coagulated state, the acid content is calculated according to e1, and if all the cyanoacrylate monomers in the three glass test tubes have flowability, the acid content is calculated according to c 1.
As a modification, in S1, the organic base is one of piperidine, pyridine or tetrabutylammonium hydroxide.
As a further improvement, in S1, the neutral organic solvent is one of dibutyl phthalate, dimethyl phthalate, ethyl cyanoacetate, or methyl cyanoacetate.
As a further improvement, in S2, the temperature in the blow-drying oven is 80 ℃.
As a further improvement, in S2, the weight ratio of the cyanoacrylate monomer to the organic base standard solution in each glass test tube is 10:1.
By adopting the technical scheme, the invention has the beneficial effects that:
according to the method for measuring the trace acid content in the cyanoacrylate adhesive, the cyanoacrylate adhesive is poor in water resistance, so that a glass test tube is firstly placed in an air-blast drying box with constant temperature of 80 ℃ to be preheated for 10min, and the glass test tube is dried, so that the influence of residual moisture in the glass test tube on content measurement is prevented.
Through multiple experiments, the concentration range of the used organic base standard solution is gradually narrowed, the content of trace acid in the cyanoacrylate adhesive is measured, and the problem that the trace acid in the cyanoacrylate adhesive is difficult to detect is solved.
After adding the organic alkali standard solution and mixing, putting the glass test tube into a blast drying oven with constant temperature of 80 ℃ again, keeping the temperature constant for 15 minutes, accelerating the curing of the cyanoacrylate adhesive by means of a certain temperature, and improving the detection efficiency.
Drawings
FIG. 1 is a sample state diagram of test tubes No. 1, no. 2 and No. 3 in example 1;
FIG. 2 is a sample state diagram of test tubes No. 4, no. 5 and No. 6 in example 1;
FIG. 3 is a sample state diagram of test tubes No. 1, no. 2 and No. 3 in example 2;
FIG. 4 is a sample state diagram of test tubes No. 4, no. 5 and No. 6 in example 2;
FIG. 5 is a sample state diagram of test tubes No. 1, no. 2 and No. 3 in example 3;
FIG. 6 is a sample state diagram of test tubes No. 4, no. 5, and No. 6 in example 3;
FIG. 7 is a sample state diagram of test tubes No. 1, no. 2 and No. 3 in example 4;
FIG. 8 is a sample state diagram of test tubes No. 4, no. 5 and No. 6 in example 4;
FIG. 9 is a sample state diagram of test tubes No. 7, no. 8, no. 9 in example 4;
FIG. 10 is a sample state diagram of test tubes No. 1, no. 2 and No. 3 in example 5;
FIG. 11 is a sample state diagram of test tubes No. 4, 5, 6 in example 5;
FIG. 12 is a sample state diagram of test tubes No. 7, no. 8, and No. 9 in example 5;
FIG. 13 is a sample state diagram of test tubes No. 1, no. 2 and No. 3 in example 6;
FIG. 14 is a sample state diagram of test tubes No. 4, 5, 6 in example 6;
FIG. 15 is a sample state diagram of test tubes No. 7, no. 8, no. 9 in example 6;
FIG. 16 is a sample state diagram of test tubes No. 1, no. 2 and No. 3 in example 7;
FIG. 17 is a sample state diagram of test tubes No. 4, 5, 6 in example 7;
FIG. 18 is a sample state diagram of test tubes No. 7, no. 8, and No. 9 in example 7;
FIG. 19 is a sample state diagram of test tubes No. 1, no. 2 and No. 3 in example 8;
FIG. 20 is a sample state diagram of test tubes No. 4, 5, 6 in example 8;
FIG. 21 is a sample state diagram of test tubes No. 7, no. 8 and No. 9 in example 8.
Detailed Description
The technical solution of the present invention will be clearly and completely described in conjunction with the specific embodiments, but it will be understood by those skilled in the art that the examples described below are some, but not all, examples of the present invention, and are intended to be illustrative only and should not be construed as limiting the scope of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The preparation method of the organic base standard mother liquor in example 1-example 2 is as follows: 1g of piperidine was dissolved in 999g of dimethyl phthalate to prepare 1000ppm of standard mother liquor of organic base.
Example 1
S1: 29g of organic base standard mother liquor is taken, 971g of dimethyl phthalate is added, and the mixture is diluted into 29ppm of organic base standard solution;
59g of organic base standard mother liquor is taken, 941g of dimethyl phthalate is added, and the mixture is diluted into 59ppm of organic base standard solution;
89g of organic alkali standard mother liquor is taken, 911g of dimethyl phthalate is added, and 89ppm of organic alkali standard solution is diluted;
s2: three glass test tubes are taken, numbered 1, 2 and 3, placed in an air blast drying oven at 80 ℃ for constant temperature preheating for 10min, then taken out, 3.0g of cyanoacrylate monomer is respectively weighed and placed in the three glass test tubes, then 0.3g of organic alkali standard solution with the concentration of 29ppm, 59ppm and 89ppm is respectively and sequentially added into the three glass test tubes 1, 2 and 3, stirring and mixing are carried out by adopting a stirring rod, the three glass test tubes are placed in the air blast drying oven at 80 ℃ again after being uniformly mixed for constant temperature for 15min, the three glass test tubes are taken out for observation after 15min, and the cyanoacrylate monomer in the glass test tube 1 is observed to have fluidity, and the cyanoacrylate monomer in the glass test tube 2 and the cyanoacrylate monomer in the glass test tube 3 are all in a solidification state as shown in figure 1;
s3: 34g of organic alkali standard mother liquor is taken, 966g of dimethyl phthalate is added, and 34ppm of organic alkali standard solution is diluted;
taking 44g of organic base standard mother liquor, adding 956g of dimethyl phthalate, and diluting to 44ppm of organic base standard solution;
taking 54g of organic base standard mother liquor, adding 946g of dimethyl phthalate, and diluting to 54ppm of organic base standard solution;
s4: three glass test tubes are taken, the serial numbers of the three glass test tubes are 4, 5 and 6, the three glass test tubes are placed in an 80 ℃ blast drying oven for constant temperature preheating for 10min, then the three glass test tubes are taken out, 3.0g of cyanoacrylate monomer is respectively weighed and placed in the three glass test tubes, then 0.3g of organic alkali standard solution with the concentration of 34ppm, 44ppm and 54ppm is respectively and sequentially added into the three glass test tubes of 4, 5 and 6, stirring and mixing are carried out by adopting a stirring rod, the three glass test tubes are placed in the 80 ℃ blast drying oven again after being uniformly mixed, the three glass test tubes are taken out for constant temperature 15min after 15min, the cyanoacrylate monomer in the No. 4 and No. 5 glass test tubes is observed to have fluidity, the cyanoacrylate monomer in the No. 6 glass test tubes is in a solidification state, and the trace acid content in the cyanoacrylate monomer is calculated as shown in fig. 2: x=0.3×54/3=5.4 ppm.
Example 2
S1: taking 28g of organic base standard mother liquor, adding 972g of dimethyl phthalate, and diluting to 28ppm of organic base standard solution;
taking 58g of organic alkali standard mother liquor, adding 942g of dimethyl phthalate, and diluting to 58ppm of organic alkali standard solution;
88g of organic alkali standard mother liquor is taken, 912g of dimethyl phthalate is added, and the mixture is diluted into 88ppm of organic alkali standard solution;
s2: three glass test tubes are taken, numbered 1, 2 and 3, placed in an 80 ℃ blast drying oven for constant temperature preheating for 10min, then taken out, respectively weighed 3.0g of cyanoacrylate monomer, placed in the three glass test tubes, respectively weighed 0.3g of organic alkali standard solution with three concentrations of 28ppm, 58ppm and 88ppm, sequentially added into the three glass test tubes 1, 2 and 3, stirred and mixed by adopting a stirring rod, the three glass test tubes are placed in the 80 ℃ blast drying oven again after uniform mixing for constant temperature for 15min, and the three glass test tubes are taken out for observation after 15min, as shown in figure 3, the cyanoacrylate monomer in the glass test tubes 1 and 2 is observed to have fluidity, and the cyanoacrylate monomer in the glass test tube 3 is in a solidification state;
s3: taking 63g of organic base standard mother liquor, adding 937g of dimethyl phthalate, and diluting to 63ppm of organic base standard solution;
taking 73g of organic base standard mother liquor, adding 927g of dimethyl phthalate, and diluting to 73ppm of organic base standard solution;
taking 83g of organic base standard mother liquor, adding 917g of dimethyl phthalate, and diluting to 83ppm of organic base standard solution;
s4: three glass test tubes are taken, the serial numbers of the three glass test tubes are 4, 5 and 6, the three glass test tubes are placed in an 80 ℃ blast drying oven for constant temperature preheating for 10min, then the three glass test tubes are taken out, 3.0g of cyanoacrylate monomer is respectively weighed and placed in the three glass test tubes, then 0.3g of organic alkali standard solution with the concentration of 63ppm, 73ppm and 83ppm is respectively and sequentially added into the three glass test tubes of 4, 5 and 6, stirring and mixing are carried out by adopting a stirring rod, after the stirring and mixing are carried out uniformly, the three glass test tubes are placed in the 80 ℃ blast drying oven again for constant temperature for 15min, after 15min, the three glass test tubes are taken out for observation, as shown in fig. 4, the cyanoacrylate monomer in the No. 4 glass test tubes is observed to have fluidity, the cyanoacrylate monomer in the No. 5 and 6 glass test tubes is in a solidification state, and the trace acid content in the cyanoacrylate monomer is calculated as follows: x=0.3×73/3=7.3 ppm.
The preparation method of the organic base standard mother liquor in example 3-example 4 is as follows: 1g of pyridine was dissolved in 999g of dibutyl phthalate to prepare 1000ppm of an organic base standard mother liquor.
Example 3
S1: taking 26g of organic base standard mother liquor, adding 974g of dibutyl phthalate, and diluting to 26ppm of organic base standard solution;
taking 56g of organic alkali standard mother liquor, adding 944g of dibutyl phthalate, and diluting to obtain 56ppm of organic alkali standard solution;
86g of organic alkali standard mother liquor is taken, 914g of dibutyl phthalate is added, and 86ppm of organic alkali standard solution is diluted;
s2: three glass test tubes are taken, numbered 1, 2 and 3, placed in an air blast drying oven at 80 ℃ for constant temperature preheating for 10min, then taken out, 3.0g of cyanoacrylate monomer is respectively weighed and placed in the three glass test tubes, then 0.3g of organic alkali standard solution with three concentrations of 26ppm, 56ppm and 86ppm is respectively and sequentially added into the three glass test tubes 1, 2 and 3, stirring and mixing are carried out by adopting a stirring rod, the three glass test tubes are placed in the air blast drying oven at 80 ℃ again after being uniformly mixed for constant temperature for 15min, the three glass test tubes are taken out for observation after 15min, and the cyanoacrylate monomer in the glass test tube No. 1 is observed to have fluidity, and the cyanoacrylate monomer in the glass test tube No. 2 and 3 is in a solidification state as shown in fig. 5;
s3: taking 31g of organic base standard mother liquor and adding 969g of dibutyl phthalate to dilute into 31ppm of organic base standard solution;
taking 41g of organic base standard mother liquor, adding 959g of dibutyl phthalate, and diluting to obtain 41ppm of organic base standard solution;
taking 51g of organic base standard mother liquor, adding 949g of dibutyl phthalate, and diluting to obtain 51ppm of organic base standard solution;
s4: three glass test tubes are taken, the serial numbers are 4, 5 and 6, the three glass test tubes are placed in an 80 ℃ blast drying oven for constant temperature preheating for 10min, then the three glass test tubes are taken out, 3.0g of cyanoacrylate monomer is respectively weighed and placed in the three glass test tubes, then 0.3g of organic base standard solution with the concentration of 31ppm, 41ppm and 51ppm is respectively and sequentially added into the three glass test tubes of 4, 5 and 6, stirring and mixing are carried out by adopting a stirring rod, the three glass test tubes are placed in the 80 ℃ blast drying oven again after being uniformly mixed, the three glass test tubes are taken out for observation after 15min, and the cyanoacrylate monomer in the No. 4, 5 and 6 glass test tubes is observed to be in a solidification state, so that the trace acid content in the cyanoacrylate monomer is calculated as shown in fig. 6: x=0.3×31/3=3.1 ppm.
Example 4
S1: taking 28g of organic base standard mother liquor, adding 972g of dibutyl phthalate, and diluting to 28ppm of organic base standard solution;
taking 58g of organic base standard mother liquor, adding 942g of dibutyl phthalate, and diluting to 58ppm of organic base standard solution;
88g of organic alkali standard mother liquor is taken, 912g of dibutyl phthalate is added, and the mixture is diluted into 88ppm of organic alkali standard solution;
s2: three glass test tubes are taken, numbered 1, 2 and 3, placed in an 80 ℃ blast drying oven for constant temperature preheating for 10min, then taken out, respectively weighed 3.0g of cyanoacrylate monomer, placed in the three glass test tubes, respectively weighed 0.3g of organic alkali standard solution with three concentrations of 28ppm, 58ppm and 88ppm, sequentially added into the three glass test tubes 1, 2 and 3, stirred and mixed by adopting a stirring rod, the three glass test tubes are placed in the 80 ℃ blast drying oven again for constant temperature 15min after being uniformly mixed, and the three glass test tubes are taken out for observation after 15min, as shown in fig. 7, the cyanoacrylate monomer in the glass test tubes 1, 2 and 3 is observed to have fluidity;
s3: 128g of organic alkali standard mother liquor is taken, 872g of dibutyl phthalate is added, and the mixture is diluted into 128ppm of organic alkali standard solution;
taking 168g of organic alkali standard mother liquor, adding 832g of dibutyl phthalate, and diluting to 168ppm of organic alkali standard solution;
taking 208g of organic base standard mother liquor, adding 792g of dibutyl phthalate, and diluting into 208ppm of organic base standard solution;
s4: three glass test tubes are taken, the serial numbers of the three glass test tubes are 4, 5 and 6, the three glass test tubes are placed in an air blast drying box at 80 ℃ for constant temperature preheating for 10min, then the three glass test tubes are taken out, 3.0g of cyanoacrylate monomer is respectively weighed and placed in the three glass test tubes, then 0.3g of organic alkali standard solution with the concentration of 128ppm, 168ppm and 208ppm is respectively and sequentially added into the three glass test tubes of 4, 5 and 6, stirring and mixing are carried out by adopting a stirring rod, after the three glass test tubes are uniformly mixed, the three glass test tubes are placed in the air blast drying box at 80 ℃ again for constant temperature for 15min, after 15min, the three glass test tubes are taken out for observation, as shown in fig. 8, the cyanoacrylate monomer in the No. 4 glass test tube and the cyanoacrylate monomer in the No. 5 glass test tube are all flowable, and the cyanoacrylate monomer in the No. 6 glass test tube is in a solidification state;
s5: taking 178g of organic alkali standard mother liquor, adding 822g of dibutyl phthalate, and diluting to 178ppm of organic alkali standard solution;
taking 188g of organic alkali standard mother liquor, adding 812g of dibutyl phthalate, and diluting to 188ppm of organic alkali standard solution;
taking 198g of organic base standard mother liquor, adding 802g of dibutyl phthalate, and diluting into 198ppm of organic base standard solution;
s6: three glass test tubes are taken, the serial numbers of the three glass test tubes are 7, 8 and 9, the three glass test tubes are placed in an air blast drying box at 80 ℃ for constant temperature preheating for 10min, then the three glass test tubes are taken out, 3.0g of cyanoacrylate monomer is respectively weighed and placed in the three glass test tubes, then 0.3g of organic alkali standard solution with three concentrations of 178ppm, 188ppm and 198ppm is respectively and sequentially added into the three glass test tubes of 7, 8 and 9, stirring and mixing are carried out by adopting a stirring rod, the three glass test tubes are placed in the air blast drying box at 80 ℃ again after being uniformly mixed, the three glass test tubes are taken out for constant temperature 15min after 15min, the cyanoacrylate monomer in the No. 7 glass test tube is observed to have fluidity, the cyanoacrylate monomer in the No. 8 and 9 glass test tubes is in a solidification state, and the trace acid content in the cyanoacrylate monomer is calculated as shown in fig. 9: x=0.3×188/3=18.8 ppm.
The preparation method of the organic base standard mother liquor in example 5-example 6 is as follows: 1g of tetrabutylammonium hydroxide was dissolved in 999g of ethyl cyanoacetate to prepare 1000ppm of an organic base standard mother liquor.
Example 5
S1: taking 28g of organic base standard mother liquor, adding 972g of ethyl cyanoacetate, and diluting to 28ppm of organic base standard solution;
taking 58g of organic base standard mother liquor, adding 942g of ethyl cyanoacetate, and diluting to 58ppm of organic base standard solution;
88g of organic alkali standard mother liquor is taken, 912g of ethyl cyanoacetate is added, and the organic alkali standard mother liquor is diluted into 88ppm of organic alkali standard solution;
s2: three glass test tubes are taken, numbered 1, 2 and 3, placed in an 80 ℃ blast drying oven for constant temperature preheating for 10min, then taken out, respectively weighed 3.0g of cyanoacrylate monomer, placed in the three glass test tubes, respectively weighed 0.3g of organic alkali standard solution with three concentrations of 28ppm, 58ppm and 88ppm, sequentially added into the three glass test tubes 1, 2 and 3, stirred and mixed by adopting a stirring rod, the three glass test tubes are placed in the 80 ℃ blast drying oven again for constant temperature 15min after being uniformly mixed, and the three glass test tubes are taken out for observation after 15min, as shown in fig. 10, the cyanoacrylate monomer in the glass test tubes 1, 2 and 3 is observed to have fluidity;
s3: 128g of organic base standard mother liquor is taken, 872g of ethyl cyanoacetate is added, and the organic base standard mother liquor is diluted into 128ppm of organic base standard solution;
168g of organic alkali standard mother liquor is taken, 832g of ethyl cyanoacetate is added, and 168ppm of organic alkali standard solution is diluted;
taking 208g of organic base standard mother liquor, adding 792g of ethyl cyanoacetate, and diluting to 208ppm of organic base standard solution;
s4: three glass test tubes are taken, the serial numbers of the three glass test tubes are 4, 5 and 6, the three glass test tubes are placed in an air blast drying box at 80 ℃ for constant temperature preheating for 10min, then the three glass test tubes are taken out, 3.0g of cyanoacrylate monomer is respectively weighed and placed in the three glass test tubes, then 0.3g of organic alkali standard solution with the concentration of 128ppm, 168ppm and 208ppm is respectively and sequentially added into the three glass test tubes of 4, 5 and 6, stirring and mixing are carried out by adopting a stirring rod, after the three glass test tubes are uniformly mixed, the three glass test tubes are placed in the air blast drying box at 80 ℃ again for constant temperature for 15min, after 15min, the three glass test tubes are taken out for observation, as shown in fig. 11, the cyanoacrylate monomer in the No. 4 glass test tubes is observed to have fluidity, and the cyanoacrylate monomer in the No. 5 and 6 glass test tubes is in a solidification state;
s5: taking 138g of organic base standard mother liquor, adding 862g of ethyl cyanoacetate, and diluting to 138ppm of organic base standard solution;
taking 148g of organic alkali standard mother liquor, adding 852g of ethyl cyanoacetate, and diluting to 148ppm of organic alkali standard solution;
taking 158g of organic base standard mother liquor, adding 842g of ethyl cyanoacetate, and diluting to 158ppm of organic base standard solution;
s6: three glass test tubes are taken, the serial numbers of the three glass test tubes are 7, 8 and 9, the three glass test tubes are placed in an 80 ℃ blast drying oven for constant temperature preheating for 10min, then the three glass test tubes are taken out, 3.0g of cyanoacrylate monomer is respectively weighed and placed in the three glass test tubes, then 0.3g of organic alkali standard solution with the concentration of 138ppm, 148ppm and 158ppm is respectively and sequentially added into the three glass test tubes of 7, 8 and 9, stirring and mixing are carried out by adopting a stirring rod, the three glass test tubes are placed in the 80 ℃ blast drying oven again after being uniformly mixed, the three glass test tubes are taken out for constant temperature 15min after 15min, and the cyanoacrylate monomer in the No. 7, 8 and 9 glass test tubes is observed to be in a solidification state, and the trace acid content in the cyanoacrylate monomer is calculated as shown in fig. 12: x=0.3×138/3=13.8 ppm.
Example 6
S1: taking 28g of organic base standard mother liquor, adding 972g of ethyl cyanoacetate, and diluting to 28ppm of organic base standard solution;
taking 58g of organic base standard mother liquor, adding 942g of ethyl cyanoacetate, and diluting to 58ppm of organic base standard solution;
88g of organic alkali standard mother liquor is taken, 912g of ethyl cyanoacetate is added, and the organic alkali standard mother liquor is diluted into 88ppm of organic alkali standard solution;
s2: three glass test tubes are taken, numbered 1, 2 and 3, placed in an 80 ℃ blast drying oven for constant temperature preheating for 10min, then taken out, respectively weighed 3.0g of cyanoacrylate monomer, placed in the three glass test tubes, respectively weighed 0.3g of organic alkali standard solution with three concentrations of 28ppm, 58ppm and 88ppm, sequentially added into the three glass test tubes 1, 2 and 3, stirred and mixed by adopting a stirring rod, the three glass test tubes are placed in the 80 ℃ blast drying oven again for constant temperature 15min after being uniformly mixed, and the three glass test tubes are taken out for observation after 15min, as shown in fig. 13, the cyanoacrylate monomer in the glass test tubes 1, 2 and 3 is observed to have fluidity;
s3: 128g of organic base standard mother liquor is taken, 872g of ethyl cyanoacetate is added, and the organic base standard mother liquor is diluted into 128ppm of organic base standard solution;
168g of organic alkali standard mother liquor is taken, 832g of ethyl cyanoacetate is added, and 168ppm of organic alkali standard solution is diluted;
taking 208g of organic base standard mother liquor, adding 792g of ethyl cyanoacetate, and diluting to 208ppm of organic base standard solution;
s4: three glass test tubes are taken, the serial numbers of the three glass test tubes are 4, 5 and 6, the three glass test tubes are placed in an 80 ℃ blast drying oven for constant temperature preheating for 10min, then the three glass test tubes are taken out, 3.0g of cyanoacrylate monomer is respectively weighed and placed in the three glass test tubes, then 0.3g of organic alkali standard solution with the concentration of 128ppm, 168ppm and 208ppm is respectively and sequentially added into the three glass test tubes of 4, 5 and 6, stirring and mixing are carried out by adopting a stirring rod, after the stirring and mixing are carried out, the three glass test tubes are placed in the 80 ℃ blast drying oven again for constant temperature for 15min, after 15min, the three glass test tubes are taken out for observation, and the cyanoacrylate monomer in the glass test tubes of 4, 5 and 6 is observed to be in a solidification state as shown in fig. 14;
s5: taking 98g of organic base standard mother liquor, adding 902g of ethyl cyanoacetate, and diluting to 98ppm of organic base standard solution;
108g of organic alkali standard mother liquor is taken, 892g of ethyl cyanoacetate is added, and the organic alkali standard mother liquor is diluted into 108ppm of organic alkali standard solution;
118g of organic base standard mother liquor is taken, 882g of ethyl cyanoacetate is added, and 118ppm of organic base standard solution is diluted;
s6: three glass test tubes are taken, the serial numbers of the three glass test tubes are 7, 8 and 9, the three glass test tubes are placed in an 80 ℃ blast drying oven for constant temperature preheating for 10min, then the three glass test tubes are taken out, 3.0g of cyanoacrylate monomer is respectively weighed and placed in the three glass test tubes, then 0.3g of organic base standard solution with three concentrations of 98ppm, 108ppm and 118ppm is respectively and sequentially added into the three glass test tubes of 7, 8 and 9, stirring and mixing are carried out by adopting a stirring rod, the three glass test tubes are placed in the 80 ℃ blast drying oven again after being uniformly mixed, the three glass test tubes are taken out for constant temperature 15min after 15min, and the cyanoacrylate monomer in the No. 7, 8 and 9 glass test tubes is observed to be in a solidification state, and the trace acid content in the cyanoacrylate monomer is calculated as shown in fig. 15: x=0.3×98/3=9.8 ppm.
The preparation method of the organic base standard mother liquor in examples 7-8 is as follows: 1g of piperidine was dissolved in 999g of methyl cyanoacetate to prepare 1000ppm of standard mother liquor of organic base.
Example 7
S1: 28g of organic base standard mother liquor is taken, 972g of methyl cyanoacetate is added, and the mixture is diluted into 28ppm of organic base standard solution;
taking 58g of organic base standard mother liquor, adding 942g of methyl cyanoacetate, and diluting to 58ppm of organic base standard solution;
88g of organic alkali standard mother liquor is taken, 912g of methyl cyanoacetate is added, and the organic alkali standard mother liquor is diluted into 88ppm of organic alkali standard solution;
s2: three glass test tubes are taken, numbered 1, 2 and 3, placed in an 80 ℃ blast drying oven for constant temperature preheating for 10min, then taken out, respectively weighed 3.0g of cyanoacrylate monomer, placed in the three glass test tubes, respectively weighed 0.3g of organic alkali standard solution with three concentrations of 28ppm, 58ppm and 88ppm, sequentially added into the three glass test tubes 1, 2 and 3, stirred and mixed by adopting a stirring rod, the three glass test tubes are placed in the 80 ℃ blast drying oven again for constant temperature 15min after being uniformly mixed, and the three glass test tubes are taken out for observation after 15min, as shown in fig. 16, the cyanoacrylate monomer in the glass test tubes 1, 2 and 3 is observed to have fluidity;
s3: 128g of organic alkali standard mother liquor is taken, 872g of methyl cyanoacetate is added, and the mixture is diluted into 128ppm of organic alkali standard solution;
168g of organic alkali standard mother liquor is taken, 832g of methyl cyanoacetate is added, and 168ppm of organic alkali standard solution is diluted;
taking 208g of organic alkali standard mother liquor, adding 792g of methyl cyanoacetate, and diluting into 208ppm of organic alkali standard solution;
s4: three glass test tubes are taken, the serial numbers of the three glass test tubes are 4, 5 and 6, the three glass test tubes are placed in an air blast drying box at 80 ℃ for constant temperature preheating for 10min, then the three glass test tubes are taken out, 3.0g of cyanoacrylate monomer is respectively weighed and placed in the three glass test tubes, then 0.3g of organic alkali standard solution with the concentration of 128ppm, 168ppm and 208ppm is respectively and sequentially added into the three glass test tubes of 4, 5 and 6, stirring and mixing are carried out by adopting a stirring rod, after the three glass test tubes are uniformly mixed, the three glass test tubes are placed in the air blast drying box at 80 ℃ again for constant temperature for 15min, after 15min, the three glass test tubes are taken out for observation, as shown in fig. 17, the cyanoacrylate monomer in the No. 4 glass test tube and the cyanoacrylate monomer in the No. 5 glass test tube are all flowable, and the cyanoacrylate monomer in the No. 6 glass test tube is in a solidification state;
s5: taking 178g of organic alkali standard mother liquor, adding 822g of methyl cyanoacetate, and diluting to 178ppm of organic alkali standard solution;
taking 188g of organic alkali standard mother liquor, adding 812g of methyl cyanoacetate, and diluting to 188ppm of organic alkali standard solution;
taking 198g of organic base standard mother liquor, adding 802g of methyl cyanoacetate, and diluting into 198ppm of organic base standard solution;
s6: three glass test tubes are taken, the serial numbers of the three glass test tubes are 7, 8 and 9, the three glass test tubes are placed in an air blast drying box at 80 ℃ for constant temperature preheating for 10min, then the three glass test tubes are taken out, 3.0g of cyanoacrylate monomer is respectively weighed and placed in the three glass test tubes, then 0.3g of organic alkali standard solution with three concentrations of 178ppm, 188ppm and 198ppm is respectively and sequentially added into the three glass test tubes of 7, 8 and 9, stirring and mixing are carried out by adopting a stirring rod, the three glass test tubes are placed in the air blast drying box at 80 ℃ again after being uniformly mixed, the three glass test tubes are taken out for constant temperature 15min after 15min, the cyanoacrylate monomer in the glass test tubes of 7 and 8 is observed to have fluidity, the cyanoacrylate monomer in the glass test tube of 9 is in a solidification state, and the trace acid content in the cyanoacrylate monomer is calculated as shown in fig. 18: x=0.3×198/3=19.8 ppm.
Example 8
S1: 28g of organic base standard mother liquor is taken, 972g of methyl cyanoacetate is added, and the mixture is diluted into 28ppm of organic base standard solution;
taking 58g of organic base standard mother liquor, adding 942g of methyl cyanoacetate, and diluting to 58ppm of organic base standard solution;
88g of organic alkali standard mother liquor is taken, 912g of methyl cyanoacetate is added, and the organic alkali standard mother liquor is diluted into 88ppm of organic alkali standard solution;
s2: three glass test tubes are taken, numbered 1, 2 and 3, placed in an 80 ℃ blast drying oven for constant temperature preheating for 10min, then taken out, 3.0g of cyanoacrylate monomer is respectively weighed and placed in the three glass test tubes, then 0.3g of organic alkali standard solution with three concentrations of 28ppm, 58ppm and 88ppm is respectively and sequentially added into the three glass test tubes 1, 2 and 3, stirring and mixing are carried out by adopting a stirring rod, after the stirring rod is carried out, the three glass test tubes are placed in the 80 ℃ blast drying oven again for constant temperature for 15min, after 15min, the three glass test tubes are taken out for observation, and as shown in fig. 19, the cyanoacrylate monomer in the glass test tubes 1, 2 and 3 is observed to have fluidity;
s3: 128g of organic alkali standard mother liquor is taken, 872g of methyl cyanoacetate is added, and the mixture is diluted into 128ppm of organic alkali standard solution;
168g of organic alkali standard mother liquor is taken, 832g of methyl cyanoacetate is added, and 168ppm of organic alkali standard solution is diluted;
taking 208g of organic alkali standard mother liquor, adding 792g of methyl cyanoacetate, and diluting into 208ppm of organic alkali standard solution;
s4: three glass test tubes are taken, the serial numbers of the three glass test tubes are 4, 5 and 6, the three glass test tubes are placed in an 80 ℃ blast drying oven for constant temperature preheating for 10min, then the three glass test tubes are taken out, 3.0g of cyanoacrylate monomer is respectively weighed and placed in the three glass test tubes, then 0.3g of organic alkali standard solution with the concentration of 128ppm, 168ppm and 208ppm is respectively and sequentially added into the three glass test tubes of 4, 5 and 6, stirring and mixing are carried out by adopting a stirring rod, after the stirring rod is carried out, the three glass test tubes are placed in the 80 ℃ blast drying oven again for constant temperature 15min after the mixing is carried out, the three glass test tubes are taken out for observation after 15min, and the cyanoacrylate monomer in the glass test tubes of 4, 5 and 6 is observed to be in a solidification state as shown in figure 20;
s5: taking 98g of organic base standard mother liquor, adding 902g of methyl cyanoacetate, and diluting to 98ppm of organic base standard solution;
108g of organic alkali standard mother liquor is taken, 892g of methyl cyanoacetate is added, and the mixture is diluted into 108ppm of organic alkali standard solution;
118g of organic alkali standard mother liquor is taken, 882g of methyl cyanoacetate is added, and 118ppm of organic alkali standard solution is diluted;
s6: three glass test tubes are taken, the serial numbers of the three glass test tubes are 7, 8 and 9, the three glass test tubes are placed in an 80 ℃ blast drying oven for constant temperature preheating for 10min, then the three glass test tubes are taken out, 3.0g of cyanoacrylate monomer is respectively weighed and placed in the three glass test tubes, then 0.3g of organic base standard solution with three concentrations of 98ppm, 108ppm and 118ppm is respectively and sequentially added into the three glass test tubes of 7, 8 and 9, stirring and mixing are carried out by adopting a stirring rod, the three glass test tubes are placed in the 80 ℃ blast drying oven again after being uniformly mixed, the three glass test tubes are taken out for constant temperature 15min after 15min, and the cyanoacrylate monomer in the No. 7, 8 and 9 glass test tubes is observed to have fluidity, and the trace acid content in the cyanoacrylate monomer is calculated as shown in figure 21: x=0.3×128/3=12.8 ppm.
The above-described embodiments of the present invention do not limit the scope of the present invention. Any other corresponding changes and modifications made in accordance with the technical idea of the present invention shall be included in the scope of the claims of the present invention.
Claims (5)
1. The method for measuring the trace acid content in the cyanoacrylate adhesive is characterized by comprising the following steps of:
s1: taking three organic alkali standard solutions a1, a2 and a3 with sequentially increasing concentrations, wherein the concentration differences between a2 and a1 and between a3 and a2 are 30ppm,25ppm is less than a1 and less than 30ppm, and the organic alkali standard solutions are prepared by dissolving organic alkali in a neutral organic solvent;
s2: the method comprises the steps of taking three glass test tubes, placing the three glass test tubes in a constant-temperature blast drying oven for preheating for 10min, taking out the three glass test tubes, respectively weighing cyanoacrylate monomers with the same quantity, placing the cyanoacrylate monomers into the three glass test tubes, respectively adding organic alkali standard solutions with the same quantity and the same concentration of a1, a2 and a3 into the three glass test tubes, stirring and mixing the three glass test tubes, placing the three glass test tubes into the constant-temperature blast drying oven again for 15min after the three glass test tubes are uniformly mixed, and taking out the three glass test tubes for first observation after 15 min;
s3: in the first observation, if one or two cyanoacrylate monomers in three glass test tubes have fluidity, the cyanoacrylate monomers in the remaining glass test tubes are in a coagulated state, three organic base standard solutions b1, b2 and b3 with sequentially increasing concentrations are taken, the concentration difference between b2 and b1 and between b3 and b2 is 10ppm, the concentration of b1 is greater than the greater concentration in the organic base standard solution for flowing the cyanoacrylate monomers, the concentration of b3 is less than the smaller concentration in the organic base standard solution for coagulating the cyanoacrylate monomers, the operation step S2 is repeated, and the second observation is performed to calculate the acid content by the smaller concentration in the organic base standard solution for coagulating the cyanoacrylate monomers, wherein the calculation formula is as follows:
X=m*A/M
wherein A is the concentration of an organic base standard solution for solidifying the cyanoacrylate monomer;
the content of acid in the X-cyanoacrylate adhesive monomer;
the mass of the m-organic alkali standard solution;
the mass of the M-cyanoacrylate adhesive monomer;
in the first observation, if all cyanoacrylate monomers in the three glass test tubes have fluidity, re-taking three organic alkali standard solutions c1, c2 and c3 with sequentially increasing concentrations, wherein the concentration of c1 is greater than that of a3, the concentration differences between c1 and a3, between c2 and c1 and between c3 and c2 are 40ppm, repeating the operation step S2, and performing the third observation;
in the third observation, if one or two of the three glass test tubes have fluidity, the cyanoacrylate monomer in the remaining glass test tubes is in a coagulated state, then taking three organic base standard solutions d1, d2 and d3 with sequentially increasing concentrations, wherein the concentration difference between d2 and d1 and between d3 and d2 is 10ppm, the concentration of d1 is larger than the larger concentration in the organic base standard solution for coagulating the cyanoacrylate monomer, the concentration of d3 is smaller than the smaller concentration in the organic base standard solution for coagulating the cyanoacrylate monomer, the difference between d1 and the larger concentration in the organic base standard solution for coagulating the cyanoacrylate monomer is 10ppm, repeating the operation step S2, and performing the fourth observation to calculate the acid content from the lower concentration in the organic base standard solution for coagulating the cyanoacrylate monomer;
in the third observation, if all the cyanoacrylate monomers in the three glass test tubes are coagulated, the three organic alkali standard solutions e1, e2 and e3 with sequentially increasing concentrations are re-taken, the concentration of e1 is larger than that of a3, the concentration of e3 is smaller than that of c1, the concentration differences between e1 and a3, between e2 and e1 and between e3 and e2 are 10ppm, and the operation step S2 is repeated, wherein in the fifth observation, one or two cyanoacrylate monomers in the glass test tubes have flowability, the cyanoacrylate monomers in the rest glass test tubes are in a coagulated state, the acid content is calculated according to the lower concentration in the organic alkali standard solution for coagulating the cyanoacrylate monomers, if all the cyanoacrylate monomers in the three glass test tubes are in a coagulated state, the acid content is calculated according to e1, and if all the cyanoacrylate monomers in the three glass test tubes have flowability, the acid content is calculated according to c 1.
2. The method for determining the trace acid content in a cyanoacrylate adhesive according to claim 1, wherein in S1, the organic base is one of piperidine, pyridine or tetrabutylammonium hydroxide.
3. The method for determining the trace acid content in the cyanoacrylate adhesive according to claim 1, wherein in S1, the neutral organic solvent is one of dibutyl phthalate, dimethyl phthalate, ethyl cyanoacetate or methyl cyanoacetate.
4. The method for measuring the trace acid content in a cyanoacrylate adhesive according to claim 1, wherein in S2, the temperature in the forced air drying oven is 80 ℃.
5. The method for determining the trace acid content in a cyanoacrylate adhesive according to claim 1, wherein in S2, a weight ratio of the cyanoacrylate monomer to the organic base standard solution in each glass test tube is 10:1.
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