CN106124693A - For measuring the method for isothiazolone content in KF88 preservative - Google Patents
For measuring the method for isothiazolone content in KF88 preservative Download PDFInfo
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- CN106124693A CN106124693A CN201610780247.9A CN201610780247A CN106124693A CN 106124693 A CN106124693 A CN 106124693A CN 201610780247 A CN201610780247 A CN 201610780247A CN 106124693 A CN106124693 A CN 106124693A
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- preservative
- isothiazolone
- hcho
- flask
- content
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- 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
Abstract
The invention provides a kind of for measuring the method for isothiazolone content in KF88 preservative, relate to content of material detection technique field, the method uses distillation equipment to substitute chromatograph/mass spectrograph, and combines chemical titration and computing formula is counter releases the content of isothiazolone in KF88 preservative.This assay method step is simple, and used detection equipment is laboratory common equipment, and detection equipment investment is little, has consumptive material low price used by higher accuracy of detection and detection process, economical and practical.
Description
Technical field
The present invention relates to content of material detection technique field, be used for measuring isothiazole in KF88 preservative particularly to one
The method of quinoline ketone content.
Background technology
KF88 preservative is also known as Kazon preservative, and activity part therein is isothiazolone compounds, isothiazolone
It is the common name of an analog derivative, predominantly 5-chloro-2-methyl-1-isothiazoline-3-ketone and 2-methyl isophthalic acid-isothiazoline-3-ketone
Mixture, wherein 5-chloro-2-methyl-1-isothiazoline-3-ketone is referred to as CMIT, 2-methyl isophthalic acid-isothiazoline-3-ketone and is called for short
MIT。
After first Goerdeler and Mittler in 1963 propose the preparation method of isothiazolone, Rohm&Hass company
Studying it always, and be used as biocide, isothiazolone has efficiently, wide spectrum, the advantage such as environmentally safe, is
A kind of ideal biocide, its market consumption is big, is widely used in petrochemical industry/daily chemical products and industrial circulation water treatment,
Current domestic many companies are also at the KF88 preservative of production and selling isothiazolone-containing.
Before this, measure isothiazolone content in KF88 preservative and generally use gas chromatography-mass spectrography or height
Effect liquid phase chromatogram (HPLC) method, although said determination method has the advantage that degree of accuracy is high, but its mensuration process needs to use
Experimental facilities expensive (mostly more than 100,000 yuan), and consumptive material used is the most cheap, if amateurish external testing machine
Structure, purchases the said equipment and consumptive material is used merely to detect the content of isothiazolone in KF88 preservative, it is clear that do not draw
Calculate.
Summary of the invention
The technical problem to be solved in the present invention be to provide a kind of accuracy of detection higher, detection equipment simple economy for surveying
Determine the method for isothiazolone content in KF88 preservative.
In order to solve above-mentioned technical problem, the present invention adopts the following technical scheme that a kind of for measuring in KF88 preservative
The method of isothiazolone content, it is characterised in that comprise the following steps:
Step one, at ambient temperature and pressure, adds distilled water, KF88 preservative sample, the phosphorus of 85% in distilling apparatus
Acid and appropriate zeolite, by described distilled water, KF88 preservative sample and the phosphoric acid mix homogeneously of 85%, described distilled water, KF88
Preservative sample and 85% the quality proportioning of phosphoric acid be 50:0.5:25.34；
Step 2, the liquid in distilling apparatus is added thermal distillation and collects distillate, when in described distilling apparatus
When liquid comes to life, in described distilling apparatus, add distilled water with the speed suitable with the described distillate rate of outflow；
Step 3, take a container, be charged with the thymol phthalein indicator of sodium sulfite solution and 0.1%, then
It is titrated to the light blue disappearance of solution, described sodium sulfite solution and the thymolphthalein of 0.1% with the sulphuric acid mark liquid of 0.25mol/L
The volume ratio of indicator is 200:1, and the content of described sodium sulfite solution sulfite sodium is 126g/L；
In step 4, the container that the whole distillates collected are proceeded in step 3, again with the sulphuric acid of 0.25mol/L
Mark liquid is titrated to the light blue disappearance of solution, the volume of the sulphuric acid mark liquid that record consumes；
Step 5, utilization calculate the percentage composition of HCHO with following formula (1), then according to the percentage composition of described HCHO,
Formula (2) is utilized instead to release the content of isothiazolone in described KF88 preservative sample:
In formula (1), V represents the volume of the sulphuric acid mark liquid consumed in described step 4；
C represents the concentration of described sulphuric acid mark liquid；
M represents the molal weight of HCHO；
M represents the quality of the KF88 preservative sample added in step one；
A represents the percentage composition of HCHO；
In formula (2), M1Represent the molal weight of isothiazolone in KF88 preservative sample；
M represents the molal weight of HCHO；
A represents the percentage composition of the HCHO calculated according to formula (1)；
B represents the percentage composition of isothiazolone in KF88 preservative sample.
Wherein, described distilling apparatus include No. 1 flask, No. 2 flasks, flask holder, electric jacket, still head, spherical condensation tube,
Constant voltage separatory funnel, No. 1 flexible pipe and No. 2 flexible pipes；
Described No. 1 flask for adding distilled water, KF88 preservative sample, the phosphoric acid of 85% and appropriate zeolite, described No. 1
In flask is placed in electric jacket and being clamped by flask holder, the bottom of described still head is inserted in the bottleneck of No. 1 flask, described steaming
The side outlet evaporating head connects spherical condensation tube entrance point, and described No. 2 flasks flow out for the port of export catching spherical condensation tube
Distillate；
Described No. 1 flexible pipe is connected with spherical condensation tube front end aperture as cooling water outlet pipe, and described No. 2 flexible pipes are as cold
But water water inlet pipe is connected with spherical condensation tube lower end aperture；
Constant voltage separatory funnel is inserted on the top of described still head.
What the present invention obtained has the beneficial effects that: the isothiazolone in KF88 preservative that is used for measuring that the present invention provides contains
The method testing procedure of amount is simple, and used detection equipment is laboratory common equipment (distilling apparatus), detects equipment investment
Little, testing result is basically identical with the detection method in background technology, has higher accuracy of detection and detection process consumption used
Material low price is economical and practical.
Detailed description of the invention
For the ease of the understanding of those skilled in the art, below in conjunction with specific embodiment, the present invention is made further
Bright.
One of the present invention is noteworthy characterized by employing distillation equipment and substitutes chromatograph/mass spectrograph, and it is next to combine formula calculating
Measure the content of isothiazolone in KF88 preservative, thus reach to reduce equipment investment and the purpose of consumptive material consumption.
Specifically, below scheme can be used to implement the present invention, one is used for measuring isothiazoline in KF88 preservative
The method of ketone content, comprises the following steps:
Step one, at ambient temperature and pressure, adds distilled water, KF88 preservative sample, the phosphorus of 85% in distilling apparatus
Acid and appropriate zeolite, by distilled water, KF88 preservative sample and the phosphoric acid mix homogeneously of 85%, distilled water, KF88 preservative sample
Product and 85% the quality proportioning of phosphoric acid be: 50:0.5:25.34；
Step 2, the liquid in distilling apparatus is added thermal distillation and collects distillate, when the liquid in distilling apparatus
When coming to life, in distilling apparatus, add distilled water with the speed suitable with the distillate rate of outflow；
Step 3, take a container, be charged with the thymol phthalein indicator of sodium sulfite solution and 0.1%, then
It is titrated to the light blue disappearance of solution, sodium sulfite solution and the thymolphthalein instruction of 0.1% with the sulphuric acid mark liquid of 0.25mol/L
The volume ratio of agent is 200:1, and the content of sodium sulfite solution sulfite sodium is 126g/L；
In step 4, the container that the whole distillates collected are proceeded in step 3, again with the sulphuric acid of 0.25mol/L
Mark liquid is titrated to the light blue disappearance of solution, the volume of the sulphuric acid mark liquid that record consumes；
Step 5, utilization calculate the percentage composition of HCHO with following formula (1), then according to the percentage composition of HCHO, utilize
The content of isothiazolone in formula (2) anti-release KF88 preservative sample:
In formula (1), V represents the volume of the sulphuric acid mark liquid consumed in step 4；
C represents the concentration of sulphuric acid mark liquid；
M represents the molal weight of HCHO；
M represents the quality of the KF88 preservative sample added in step one；
A represents the percentage composition of HCHO；
In formula (2), M1Represent the molal weight of isothiazolone in KF88 preservative sample；
M represents the molal weight of HCHO；
A represents the percentage composition of the HCHO calculated according to formula (1)；
B represents the percentage composition of isothiazolone in KF88 preservative sample.
In the above-described embodiments, it is preferred that distilling apparatus includes No. 1 flask, No. 2 flasks, flask holder, electric jacket, distillations
Head, spherical condensation tube, constant voltage separatory funnel, No. 1 flexible pipe and No. 2 flexible pipes；
No. 1 flask is for adding distilled water, KF88 preservative sample, the phosphoric acid of 85% and appropriate zeolite, and No. 1 flask is placed in
In electric jacket and being clamped by flask holder, the bottom of still head is inserted in the bottleneck of No. 1 flask, and the side outlet of still head is even
Connect spherical condensation tube entrance point, the distillate that No. 2 flasks flow out for the port of export catching spherical condensation tube；
No. 1 flexible pipe is connected with spherical condensation tube front end aperture as cooling water outlet pipe, and No. 2 flexible pipes are as cooling water water inlet
Pipe is connected with spherical condensation tube lower end aperture；
Constant voltage separatory funnel is inserted on the top of still head.
It should be noted that in the above-described embodiments, No. 1 flask used in distilling apparatus, No. 2 flasks, flask holder, electricity
Hot jacket, still head, spherical condensation tube, constant voltage separatory funnel, No. 1 flexible pipe and No. 2 flexible pipes are well known in the prior art general
Structure, the present invention is not related to the improvement to above-mentioned experiment equipment, and the connected mode between above-mentioned equipment is relatively simple, passes through
Above word describes, and those skilled in the art can be best appreciated the connection knot in distilling apparatus between each parts
Structure, therefore the present invention does not reoffer the attachment structure figure of this distilling apparatus.
The distilling apparatus that use above preferred structure is described below to measure isothiazolone content in KF88 preservative
Operational approach.
Step one, at ambient temperature and pressure, adds distilled water 50g (50ml), KF88 preservative sample in No. 1 flask
0.5g, the phosphoric acid 25.34g (15ml) of 85% and 1-2 zeolite, shake the phosphoric acid of distilled water, KF88 preservative sample and 85%
Even, in constant voltage separatory funnel, add distilled water 200ml, and by leather plug, mouth is stoppered；
Step 2, unlatching electric jacket add thermal distillation and collect distillation by No. 2 flasks the liquid in No. 1 flask
Liquid, when the liquid in No. 1 flask comes to life, opens the switch of constant voltage separatory funnel, with suitable with the distillate rate of outflow
Speed toward No. 1 flask adds distilled water；
Step 3, take a conical flask, be charged with 30ml sodium sulfite solution and the hundred of 3 (about 0.15ml) 0.1%
In fragrant phenolphthalein indicator, be then titrated to the light blue disappearance of solution, above-mentioned sodium sulfite solution with the sulphuric acid mark liquid of 0.25mol/L
The content of sulfite sodium is 126g/L；
In step 4, the taper that the whole distillates collected in No. 2 flasks are proceeded in step 3, again use
The sulphuric acid mark liquid of 0.25mol/L is titrated to the light blue disappearance of solution, the volume of the sulphuric acid mark liquid that record consumes；
Step 5, utilization calculate the percentage composition of HCHO with following formula (1), then according to the percentage composition of HCHO, utilize
The content of isothiazolone in formula (2) anti-release KF88 preservative sample:
In formula (1), V represents the volume of the sulphuric acid mark liquid consumed in step 4；
C represents the concentration of sulphuric acid mark liquid；
M represents the molal weight of HCHO；
M represents the quality of the KF88 preservative sample added in step one；
A represents the percentage composition of HCHO；
In formula (2), M1Represent the molal weight of isothiazolone in KF88 preservative sample；
M represents the molal weight of HCHO；
A represents the percentage composition of the HCHO calculated according to formula (1)；
B represents the percentage composition of isothiazolone in KF88 preservative sample.
For verifying the accuracy of said determination method, applicant choose commercially available a kind of KF88 preservative (model: DL604,
Wherein isothiazolone actual content is 2%) use said method and gas chromatography-mass spectrography respectively to isothiazoline therein
Ketone content is measured, the method provided through the present invention record wherein isothiazolone content be 1.985% (for improving precision,
After in test process, in each step, the addition of related substances is accurate to arithmetic point three), through high performance liquid chromatography (HPLC) method
Recording wherein isothiazolone content is 2.010%, it is seen from the above data that the assay method of present invention offer and gas phase
Chromatography mass spectrometry testing result closely, thus it was determined that the present invention provide assay method also there is higher detection
Precision.
Above-described embodiment is the present invention preferably implementation, and in addition, the present invention can realize with alternate manner,
On the premise of conceiving without departing from the technical program, any obvious replacement is all within protection scope of the present invention.
Finally it should be emphasised that, in order to allow those of ordinary skill in the art understand more easily, the present invention is relative to existing
Having the improvements of technology, some descriptions of the present invention have been simplified, and for clarity sake, present specification is omitted
Some other elements, those of ordinary skill in the art it is to be appreciated that these elements omitted also may make up present disclosure.
Claims (2)
1. one kind is used for measuring the method for isothiazolone content in KF88 preservative, it is characterised in that comprise the following steps:
Step one, at ambient temperature and pressure, add in distilling apparatus distilled water, KF88 preservative sample, the phosphoric acid of 85% and
Appropriate zeolite, by described distilled water, KF88 preservative sample and the phosphoric acid mix homogeneously of 85%, described distilled water, KF88 anticorrosion
Agent sample and 85% the quality proportioning of phosphoric acid be: 50:0.5:25.34；
Step 2, the liquid in distilling apparatus is added thermal distillation and collects distillate, the liquid in described distilling apparatus
When coming to life, in described distilling apparatus, add distilled water with the speed suitable with the described distillate rate of outflow；
Step 3, take a container, be charged with the thymol phthalein indicator of sodium sulfite solution and 0.1%, then use
The sulphuric acid mark liquid of 0.25mol/L is titrated to the light blue disappearance of solution, described sodium sulfite solution and 0.1% thymolphthalein refer to
The volume ratio showing agent is 200:1, and the content of described sodium sulfite solution sulfite sodium is 126g/L；
In step 4, the container that the whole distillates collected are proceeded in step 3, again with the sulphuric acid mark liquid of 0.25mol/L
It is titrated to the light blue disappearance of solution, the volume of the sulphuric acid mark liquid that record consumes；
Step 5, utilization calculate the percentage composition of HCHO with following formula (1), then according to the percentage composition of described HCHO, utilize
The content of isothiazolone in formula (2) the anti-described KF88 preservative sample of release:
In formula (1), V represents the volume of the sulphuric acid mark liquid consumed in described step 4；
C represents the concentration of described sulphuric acid mark liquid；
M represents the molal weight of HCHO；
M represents the quality of the KF88 preservative sample added in step one；
A represents the percentage composition of HCHO；
In formula (2), M1Represent the molal weight of isothiazolone in KF88 preservative sample；
M represents the molal weight of HCHO；
A represents the percentage composition of the HCHO calculated according to formula (1)；
B represents the percentage composition of isothiazolone in KF88 preservative sample.
It is the most according to claim 1 for measuring the method for isothiazolone content in KF88 preservative, it is characterised in that:
Described distilling apparatus includes No. 1 flask, No. 2 flasks, flask holder, electric jacket, still head, spherical condensation tube, constant voltage separatory
Funnel, No. 1 flexible pipe and No. 2 flexible pipes；
Described No. 1 flask is for adding distilled water, KF88 preservative sample, the phosphoric acid of 85% and appropriate zeolite, described No. 1 flask
In being placed in electric jacket and being clamped by flask holder, the bottom of described still head is inserted in the bottleneck of No. 1 flask, described still head
Side outlet connect spherical condensation tube entrance point, described No. 2 flasks for catch spherical condensation tube the port of export flow out steaming
Distillate；
Described No. 1 flexible pipe is connected with spherical condensation tube front end aperture as cooling water outlet pipe, and described No. 2 flexible pipes are as cooling water
Water inlet pipe is connected with spherical condensation tube lower end aperture；
Constant voltage separatory funnel is inserted on the top of described still head.
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