CN103852536A - Detecting method for organic tin in plastic component of electronic element - Google Patents
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Abstract
The invention discloses a detecting method for organic tin in a plastic component of an electronic element. The detecting method comprises the following steps of (a) treating a sample to form particles, wherein the length and width of each particle are respectively not larger than 0.5cm; (b) placing the sample treated in the step (a) into n-hexane to carry out ultrasonic vibration, then, adding sodium acetate to carry out ultrasonic vibration, and next, cooling to the room temperature, wherein the ratio of the sample to a solvent is 1: (5-20)g/mL; (c) adding a derivating agent Tetraethylborate and vibrating, wherein the ratio of the addition quantity of the derivating agent to the quantity of the sample is (02-1):1mL/g; (d) analyzing the solution extracted in the step (c) by using a GC-MS (Gas Chromatography-Mass Spectrometer), and setting a special chromatographic condition. The analysis method provided by the invention is rapid and good in repeatability and reproducibility.
Description
Technical field
The present invention relates to a kind of detection method of organotin, relate in particular to the detection method of organotin in a kind of electronic devices and components plastic components.
Background technology
Organo-tin compound is tin and the carbon metal organic compound that directly combination forms.General formula R nSnX4-n(n=1-4, R is alkyl or aromatic radical).There are Alkyzin compound and compound aromatic base two classes.Its basic structure has a replacement body, two to replace body, three replacement bodies and four replace bodies (referring to the number of R).10-20% in tin output is for the synthesis of organo-tin compound.Organotin can be used as the coating of catalyzer, stabilizing agent (as stannous methide, dioctyl tin, tetraphenyltin), agricultural insecticide, germifuge (as dibutyl tin, tributyl tin, triphenyltin) and articles for daily use and mildewproof agent, plastics are medium.
In physical environment, the effect of organo-tin compound and heat, light, water, oxygen, ozone etc., can decompose rapidly.Enter after biosome, small intestine or skin easily absorb, and particularly three replacement bodies are the most easily absorbed, and are distributed in liver, kidney and brain.The speed that takes off alkyl, de-aromatic radical in body take liver as main microsome drug metabolizing system is very fast.Organo-tin compound to the main infringement of biosome is: central nervous system can cause oxidative phosphorylation process in Leukoedema, cellular energy utilization to be subject to barrier, thymus gland and lymphoid inhibiting effect, cellular immunity to be subject to impairment, hormone secretion to suppress to cause diabetes and high fat of blood etc.To people's toxicity, the local spread effect to skin, respiratory tract, cornea, can cause that by skin or encephaledema whole body is poisoning, even dead.
The tin alkyl of separate constituent or phenyltin analytical approach have many reports, and the method for simultaneously analyzing has following three kinds: (1) direct method: the GC-ECD of souring soln injection is in advance tested.Make post passivation, be adjusted to after certain state, the sample extracting, purify is injected to GC and carry out quantitatively.(2) reducing process: in sample solution, haloalkyl tin is in advance with sodium borohydride reduction, generation tin alkyl hydride GC-ECD or GC-FPD separation and quantitative.(3) tetraalkyl method: it is quantitative by GC-FPD that haloalkyl tin becomes tetraalkyl tin by the alkylation of Grignard reagent.
But the detection method of the organotin in parts material of repeatability and accuracy mould to(for) electronic devices and components need further improvement.
Summary of the invention
The object of the present invention is to provide the detection method of organotin in a kind of electronic devices and components.Whether method of the present invention is by selecting suitable solvent by sample ultrasonic ripple concussion extraction, makes organotin extracting substances wherein to solution, then carry out in analytic sample containing organotin and content thereof with GC-MS.Show through large quantity research, method accuracy of the present invention is high, repeatability and repeatability excellence.
For reaching above-mentioned purpose, the present invention by the following technical solutions:
In electronic devices and components, a detection method for organotin, comprises the steps:
(a) sample preparation is become to be not more than 0.5cm*0.5cm, as the particle of 0.3cm*0.4cm, 0.2cm*0.5cm, 0.3cm*0.3cm etc.;
(b) step (a) sample after treatment is put into normal hexane and carry out ultrasonic oscillation, and then be cooled to room temperature after adding sodium acetate ultrasonic oscillation; The ratio of sample and solvent is 1:5-20g/mL, for example, be 1:7g/mL, 1:10g/mL, 1:14g/mL, 1:18g/mL etc.;
(c) add derivating agent tetraethyl sodium borate, concussion; Adding the amount of derivating agent and the ratio of sample is 0.2-1:1mL/g, for example, be 0.4:1g/mL, 0.6:1g/mL, 0.9:1g/mL etc.;
(d) step (c) gained solution is carried out to GC-MS analysis;
Wherein, the chromatographic column of GC-MS is low pole, be for example OV-5, DB-5, SE-54, HP-5, RTX-5, BP-5 etc., when GC-MS analyzes, the temperature programmed control of GC part is set to: initial temperature 40-60 ℃, being for example 43 ℃, 46 ℃, 52 ℃ etc. and keeping 0.5-2min, for example, is 0.7min, 1.5min etc.; With 10-15 ℃/min, be for example that 11 ℃/min, 14 ℃/min etc. rise to 140-160 ℃, it is for example 145 ℃, 153 ℃, 158 ℃ etc., again with 5-10 ℃/min, be for example that 7 ℃/min, 9 ℃/min rise to 260-270 ℃, being for example 263 ℃, 269 ℃ etc., more than keeping 5min, for example, is 7min, 12min, 15min etc.
Carrying out before GC-MS quantitative test, first use GC-MS to carry out qualitative analysis to sample, determine whether the organotin that contains organotin and contain which type, the type of the organotin then containing in is per sample prepared corresponding standard solution and is carried out quantitative test.
The present invention by a large amount of determined use ultrasonic extraction then carry out that GC-MS analyzes can be accurate, obtain reliably the content of the organotin in electronic devices and components, wherein choosing of ultrasonic extraction solvent has important impact to the extraction completely of organotin, can better organotin be extracted from product, solvent selects and accuracy to analysis result of the setting of chromatographic condition and repeatability, repeatability have material impact.
As optimization technique method, detection method of the present invention, the ratio of described sample and solvent is 1:10g/mL, adding the amount of derivating agent and the ratio of sample is 0.5:1mL/g.
As optimization technique method, detection method of the present invention, in step (b), the condition of ultrasonic oscillation is: more than shaking 40min at 50-80 ℃, pressure release 2～15min for the first time, pressure release 10～40min for the second time, for the third time more than pressure release 30min; Preferably, shake 60min, pressure release 5～10min for the first time, pressure release 15～25min for the second time, for the third time pressure release 45min at 70 ℃.
Preferably, add the condition of sodium acetate concussion to be: more than shaking 20min at 50-80 ℃, preferably to shake 30min at 70 ℃.
As optimization technique method, detection method of the present invention, adds the condition of derivating agent concussion to be: more than jolting 20min with the above speed of 200rpm, preferably, to jolt 30min with 250rpm speed in step (c).
As optimization technique method, detection method of the present invention, the chromatographic column of GC-MS is DB-5, and length is 30m, and internal diameter is 0.25mm, and thickness is 0.25 μ m.
Preferably, carrier gas when GC-MS analyzes is helium, and flow is 0.7-1.5mL/min, be for example 0.9mL/min, 1.3mL/min etc., be preferably 1mL/min, adopt split sampling, injection temperature is 270-290 ℃, for example, be 275 ℃, 283 ℃, 288 ℃ etc., is preferably 280 ℃.
As optimization technique method, detection method of the present invention, when GC-MS analyzes, the temperature programmed control of GC part is set to: 50.0 ℃ of maintenance 1.00min of initial temperature; Rise to 160 ℃ with 12.0 ℃/min, then rise to 265 ℃ with 8.0 ℃/min, keep 7.00min.
As optimization technique method, detection method of the present invention, when GC-MS analyzes, the condition setting of MS part is: interface temperature 230-270 ℃, it is for example 240 ℃, 260 ℃, 268 ℃ etc., source temperature 200-230 ℃, for example, be 210 ℃, 222 ℃ etc., sweep limit 50 to 450amu; 250 ℃ of preferable interface temperature, 220 ℃ of source temperature, sweep limit 50 is to 450amu.
The testing conditions that the present invention sets can make detection material separate, and makes quantitative result more accurate.
As optimization technique method, detection method of the present invention, comprises the steps:
(a) sample preparation is become to be not more than the particle of 0.5cm*0.5cm;
(b) more than step (a) sample after treatment put into being carried out ultrasonic oscillation 40min at normal hexane 50-80 ℃, pressure release 2～15min for the first time, pressure release 10～40min for the second time, for the third time more than pressure release 30min, and then be cooled to room temperature after adding at sodium acetate 50-80 ℃ ultrasonic oscillation 20min above; The ratio of sample and solvent is 1:5-20g/mL;
(c) add derivating agent tetraethyl sodium borate, more than jolting 20min with the above speed of 200rpm; Adding the amount of derivating agent and the ratio of sample is 0.2-1:1mL/g;
(d) solution after step (c) extraction is carried out to GC-MS analysis; The chromatographic column of GC-MS is low pole; Carrier gas when GC-MS analyzes is helium, and flow is 0.7-1.5mL/min, adopts split sampling, and injection temperature is 270-290 ℃; The temperature programmed control of GC part is set to: initial temperature 40-60 ℃ keeps 0.5-2min; Rise to 140-160 ℃ with 10-15 ℃/min, then rise to 260-270 ℃ with 5-10 ℃/min, more than keeping 5min; The condition setting of MS part is: interface temperature 230-270 ℃, and source temperature 200-230 ℃, sweep limit 50 is to 450amu.
As optimization technique method, detection method of the present invention, comprises the steps:
(a) sample preparation is become to be not more than the particle of 0.5cm*0.5cm;
(b) step (a) sample after treatment is put at 70 ℃ of normal hexanes and carried out ultrasonic oscillation 60min, pressure release 5～10min for the first time, pressure release 15～25min for the second time, pressure release 45min for the third time, and then add at 70 ℃ of sodium acetates and be cooled to room temperature after ultrasonic oscillation 30min; The ratio of sample and solvent is 1:10g/mL;
(c) add derivating agent tetraethyl sodium borate, jolt 30min with 250rpm speed; Adding the amount of derivating agent and the ratio of sample is 0.5:1mL/g;
(d) solution after step (c) extraction is carried out to GC-MS analysis; The chromatographic column of GC-MS is DB-5, length 30m, internal diameter 0.25mm, thickness 0.25 μ m; Carrier gas when GC-MS analyzes is helium, and flow is 1mL/min, adopts split sampling, and injection temperature is 280 ℃; The temperature programmed control of GC part is set to: 50.0 ℃ of maintenance 1.00min of initial temperature; Rise to 160 ℃ with 12.0 ℃/min, then rise to 265 ℃ with 8.0 ℃/min, keep 7.00min; The condition setting of MS part is: 250 ℃ of interface temperature, and 220 ℃ of source temperature, sweep limit 50 is to 450amu.
Detection method of the present invention is easy, quick, and accuracy is high, repeatability and repeatability good.
The present invention is described in more detail below.But following example is only simple and easy example of the present invention, does not represent or limit the scope of the present invention, and protection scope of the present invention is as the criterion with claims.
Embodiment
For the present invention is described better, be convenient to understand technical scheme of the present invention, typical but non-limiting embodiment of the present invention is as follows.
Instrument equipment in embodiment:
Quantitatively test tube, GC-MS analyzes with bottle (2ml), transfer pipet (1ml, 10ml), 100 μ l entry needles, safe rubber pipette bulb, electronic balance (degree of accuracy 0.01mg), ultrasonic oscillation device;
Gas chromatography mass spectrometer GC/MS, chromatographic column: Column (DB-5) length 30m, internal diameter 0.25mm, thickness 0.25 μ m, resistance to extreme temperature: 350 ℃.
Agents useful for same in embodiment:
Normal hexane, CH3 (CH2) 4CH3, M.W=86;
Sodium acetate, CH3COONa, M.W=82,1M, collocation method: get 4.1g sodium acetate and be added in 40ml deionized water, first add acetic acid 1.75ml, be more slowly transferred to pH value to 4.5 with acetic acid, finally quantitatively arrive 50ml;
Derivating agent, tetraethyl sodium borate, collocation method: get 0.5g Tetraethylborate and be added in THF, last quantitatively to 10ml (this liquid needs configuration on the same day);
Standard items STD:(is dissolved in methyl alcohol)
DBT (stannous phenide chloride, (C4H9) 2SnCl2, M.W=304)
TBT (triphenyltin chloride, (C4H9) 3SnCl, M.W=325.5)
First each standard items are mixed with to 1000ppm, called after numbering A (get each standard items of 100mg to the volume bottle of same bottle 100ml, add methyl alcohol and be diluted to groove).Dilute according to following table 1 again:
Table 1
Embodiment 1
(a) be cut into the particle of 0.5*0.5cm size with electronics capacity of balance sample wire strip diode plastic components 1.0085g, put into Boiling tube, add the hexane of 10ml;
(b) ultrasonic vibrating 1 hour (70 ℃), pressure release 5min for the first time, pressure release 25min for the second time, for the third time pressure release 45min; Add sodium acetate 10ml, with 70 ℃ concussion 30min, after be cooled to room temperature;
(c) add derivating agent 0.5ml, jolt 30min with 250rpm;
(d) solution is poured out, got upper solution 1ml to the upper machine analysis of bottle (vial).
GC part condition:
Injection system: shunting (Split), at 1.00min, SPL1 is set as 5; Injection temperature: 280 ℃; Portable gas: adjusting its flow with He is 1ml/min;
Temperature programmed control: 50.0 ℃ of maintenance 1.00min of initial temperature, are warming up to 150 ℃ with 12.0 ℃/min, then are warming up to 265 ℃ of maintenance 7.00min with 8.0 ℃/min;
MS part condition: 250 ℃ of interface temperature, 220 ℃ of source temperature, sweep limit: 50 to 450amu.
The calibration curve making of AU1～AU5, recording organotin concentration in sample solution is 11ng/ml, in sample, organotin content is 0.2236mg/kg.Get 10 parts of same samples respectively through shredding, extract post analysis, the content obtaining in final sample is 0.2236mg/kg, 0.2207mg/kg, 0.2289mg/kg, 0.2278mg/kg, 0.2199mg/kg, 0.2276mg/kg, 0.2307mg/kg, 0.2256mg/kg, 0.2267mg/kg, 0.2198mg/kg, the relative standard deviation of ten test results is 1.74%, and the repeatability of visible this method is fine.Carry out repeatability test result by 5 laboratories respectively for same sample as follows: 0.2251mg/kg, 0.2344mg/kg, 0.2314mg/kg, 0.2146mg/kg, 0.2237mg/kg, the relative standard deviation of the test result of 5 different experiments chambers is 3.40%, visible, method of testing of the present invention has also obtained extraordinary repeatability between different laboratories.The test of carrying out recovery of standard addition records the recovery between 98-103%, and visible detection method of the present invention has higher accuracy.
Embodiment 2
(a) be cut into the particle of 0.3*0.3cm size with electronics capacity of balance sample wire strip resistance plastic components 1.0145g, put into Boiling tube, add the hexane of 5ml;
(b) ultrasonic vibrating 40min (80 ℃), pressure release 10min for the first time, pressure release 15min for the second time, for the third time pressure release 30min; Add sodium acetate 15ml, with 80 ℃ concussion 50min, after be cooled to room temperature;
(c) add derivating agent 1ml, jolt 20min with 250rpm;
(d) solution is poured out, got upper solution 1ml to the upper machine analysis of bottle (vial).
GC part condition:
Injection system: shunting (Split), at 1.00min, SPL1 is set as 5; Injection temperature: 270 ℃; Portable gas: adjusting its flow with He is 0.7ml/min;
Temperature programmed control: 45.0 ℃ of maintenance 2.00min of initial temperature, are warming up to 160 ℃ with 10.0 ℃/min, then are warming up to 270 ℃ of maintenance 10.00min with 5.0 ℃/min;
MS part condition: 230 ℃ of interface temperature, 200 ℃ of source temperature, sweep limit: 50 to 450amu.
The calibration curve making of AU1～AU5, recording organotin concentration in sample solution is 36ng/ml, in sample, organotin content is 0.7452mg/g.Get 10 parts of same samples respectively through shredding, extract post analysis, the content obtaining in final sample is 0.7452mg/kg, 0.7414mg/kg, 0.7509mg/kg, 0.7433mg/kg, 0.7233mg/kg, 0.7321mg/kg, 0.7444mg/kg, 0.7503mg/kg, 0.7410mg/kg, 0.7398mg/kg, the relative standard deviation of ten test results is 1.11%, and the repeatability of visible this method is fine.Carry out repeatability test result by 5 laboratories respectively for same sample as follows: 0.7412mg/kg, 0.7356mg/kg, 0.7562mg/kg, 0.7478mg/kg, 0.6869mg/kg, the relative standard deviation of the test result of 5 different experiments chambers is 3.71%, visible, method of testing of the present invention has also obtained extraordinary repeatability between different laboratories.
Applicant's statement, person of ordinary skill in the field is on the basis of above-described embodiment, by the concrete content point value of above-described embodiment component, combined with the technical scheme of summary of the invention part, thereby the new numerical range producing, also be one of record scope of the present invention, the application, for making instructions simple and clear, is no longer enumerated these numerical ranges.
Applicant's statement, the present invention illustrates manufacture craft of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned making step, does not mean that the present invention must rely on above-mentioned making step and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, and the selections of the equivalence replacement to the selected raw material of the present invention and the interpolation of auxiliary element, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characterictic described in above-mentioned embodiment, in reconcilable situation, can combine by any suitable mode, for fear of unnecessary repetition, the present invention is to the explanation no longer separately of various possible array modes.
In addition, also can carry out combination in any between various embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (9)
1. a detection method for organotin in electronic devices and components plastic components, comprises the steps:
(a) sample preparation is become to be not more than the particle of 0.5cm*0.5cm;
(b) step (a) sample after treatment is put into normal hexane and carry out ultrasonic oscillation, and then be cooled to room temperature after adding sodium acetate ultrasonic oscillation; The ratio of sample and solvent is 1:5-20g/mL;
(c) add derivating agent tetraethyl sodium borate, concussion; Adding the amount of derivating agent and the ratio of sample is 0.2-1:1mL/g;
(d) step (c) gained solution is carried out to GC-MS analysis;
Wherein, the chromatographic column of GC-MS is low pole, and when GC-MS analyzes, the temperature programmed control of GC part is set to: initial temperature 40-60 ℃ keeps 0.5-2min; Rise to 140-160 ℃ with 10-15 ℃/min, then rise to 260-270 ℃ with 5-10 ℃/min, more than keeping 5min.
2. detection method as claimed in claim 1, is characterized in that, the ratio of described sample and solvent is 1:10g/mL, and adding the amount of derivating agent and the ratio of sample is 0.5:1mL/g.
3. detection method as claimed in claim 1, it is characterized in that, in step (b), the condition of ultrasonic oscillation is: more than shaking 40min at 50-80 ℃, and pressure release 2～15min for the first time, pressure release 10～40min for the second time, for the third time more than pressure release 30min; Preferably, shake 60min, pressure release 5～10min for the first time, pressure release 15～25min for the second time, for the third time pressure release 45min at 70 ℃;
Preferably, add the condition of sodium acetate concussion to be: more than shaking 20min at 50-80 ℃, preferably to shake 30min at 70 ℃.
4. the detection method as described in claim 1-3 any one, is characterized in that, adds the condition of derivating agent concussion to be: more than jolting 20min with the above speed of 200rpm, preferably, to jolt 30min with 250rpm speed in step (c).
5. the detection method as described in claim 1-4 any one, is characterized in that, the chromatographic column of GC-MS is DB-5, and length is 30m, and internal diameter is 0.25mm, and thickness is 0.25 μ m;
Preferably, carrier gas when GC-MS analyzes is helium, and flow is 0.7-1.5mL/min, is preferably 1mL/min, adopts split sampling, and injection temperature is 270-290 ℃, is preferably 280 ℃.
6. the detection method as described in claim 1-5 any one, is characterized in that, when GC-MS analyzes, the temperature programmed control of GC part is set to: 50.0 ℃ of maintenance 1.00min of initial temperature; Rise to 160 ℃ with 12.0 ℃/min, then rise to 265 ℃ with 8.0 ℃/min, keep 7.00min.
7. the detection method as described in claim 1-6 any one, is characterized in that, when GC-MS analyzes, the condition setting of MS part is:; Interface temperature 230-270 ℃, source temperature 200-230 ℃, sweep limit 50 is to 450amu; Be preferably 250 ℃ of interface temperature, 220 ℃ of source temperature, sweep limit 50 is to 450amu.
8. detection method as claimed in claim 1, is characterized in that, comprises the steps:
(a) sample preparation is become to be not more than the particle of 0.5cm*0.5cm;
(b) more than step (a) sample after treatment put into being carried out ultrasonic oscillation 40min at normal hexane 50-80 ℃, pressure release 2～15min for the first time, pressure release 10～40min for the second time, for the third time more than pressure release 30min, and then be cooled to room temperature after adding at sodium acetate 50-80 ℃ ultrasonic oscillation 20min above; The ratio of sample and solvent is 1:5-20g/mL;
(c) add derivating agent tetraethyl sodium borate, more than jolting 20min with the above speed of 200rpm; Adding the amount of derivating agent and the ratio of sample is 0.2-1:1mL/g;
(d) solution after step (c) extraction is carried out to GC-MS analysis; The chromatographic column of GC-MS is low pole; Carrier gas when GC-MS analyzes is helium, and flow is 0.7-1.5mL/min, adopts split sampling, and injection temperature is 270-290 ℃; The temperature programmed control of GC part is set to: initial temperature 40-60 ℃ keeps 0.5-2min; Rise to 140-160 ℃ with 10-15 ℃/min, then rise to 260-270 ℃ with 5-10 ℃/min, more than keeping 5min; The condition setting of MS part is: interface temperature 230-270 ℃, and source temperature 200-230 ℃, sweep limit 50 is to 450amu.
9. detection method as claimed in claim 1, is characterized in that, comprises the steps:
(a) sample preparation is become to be not more than the particle of 0.5cm*0.5cm;
(b) step (a) sample after treatment is put at 70 ℃ of normal hexanes and carried out ultrasonic oscillation 60min, pressure release 5～10min for the first time, pressure release 15～25min for the second time, pressure release 45min for the third time, and then add at 70 ℃ of sodium acetates and be cooled to room temperature after ultrasonic oscillation 30min; The ratio of sample and solvent is 1:10g/mL;
(c) add derivating agent tetraethyl sodium borate, jolt 30min with 250rpm speed; Adding the amount of derivating agent and the ratio of sample is 0.5:1mL/g;
(d) solution after step (c) extraction is carried out to GC-MS analysis; The chromatographic column of GC-MS is DB-5, length 30m, internal diameter 0.25mm, thickness 0.25 μ m; Carrier gas when GC-MS analyzes is helium, and flow is 1mL/min, adopts split sampling, and injection temperature is 280 ℃; The temperature programmed control of GC part is set to: 50.0 ℃ of maintenance 1.00min of initial temperature; Rise to 160 ℃ with 12.0 ℃/min, then rise to 265 ℃ with 8.0 ℃/min, keep 7.00min; The condition setting of MS part is: 250 ℃ of interface temperature, and 220 ℃ of source temperature, sweep limit 50 is to 450amu.
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| CN115078605A (en) * | 2022-06-15 | 2022-09-20 | 宁波中普检测技术服务有限公司 | Method for detecting isooctyl thioglycolate di-n-octyl tin in polyvinyl chloride plastic |
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