CN106124690A - Indirect iodometric processes measures the method for antimony content in methyl stannum antimony composite thermal stabilizer - Google Patents
Indirect iodometric processes measures the method for antimony content in methyl stannum antimony composite thermal stabilizer Download PDFInfo
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- CN106124690A CN106124690A CN201610445414.4A CN201610445414A CN106124690A CN 106124690 A CN106124690 A CN 106124690A CN 201610445414 A CN201610445414 A CN 201610445414A CN 106124690 A CN106124690 A CN 106124690A
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Abstract
The present invention relates to indirect iodometric processes and measure the method for antimony content in methyl stannum antimony composite thermal stabilizer, comprise the following steps: (1) weighs a certain amount of methyl stannum antimony composite thermal stabilizer sample, being sequentially added into concentrated sulphuric acid, concentrated nitric acid and perchloric acid, three kinds of sour volume ratios are 2～3:1:1, and sample quality is 1:35～55 with the ratio of mixed acid volume, g/ml, heating for dissolving, treats that it is cooled to room temperature and adds (1+9) hydrochloric acid solution constant volume, and the volume of constant volume is V, shake up, standby；(2) pipetting volume is V0Step (1) prepare solution, add appropriate potassium iodide and starch indicator, the sodium thiosulfate standard titration solution utilizing molar concentration 1.000mol/L titrates, and becomes colorless as titration end-point, the volume V of record consumption sodium thiosulfate standard titration solution to solution blueness1, doing blank assay simultaneously and writing down volume is V2, by formula 1:
Description
Technical field
The present invention relates to the assay method of a kind of PVC methyl stannum antimony composite thermal stabilizer antimony content, more particularly to
A kind of indirect iodometric processes measures the method for antimony content in methyl stannum antimony composite thermal stabilizer.
Background technology
Granted patent ZL201010254909.1 of Zhejiang Hai Pudun new material limited company application is by compounding skill
Art is prepared for a kind of methyl stannum antimony liquid composite thermal stabilizer, and it is mainly composed of thiol methyl tin, mercaptans type and auxiliary addition agent.
Product improves initial stage of PVC product and long-term thermal stability and goods transparency, improves the processing rheological property of PVC product,
Extend manufacture cycle, protect equipment, reduce the Theil indices in methyl tin heat stabilizer, reduce consumption and the dirt thereof of rare metal stannum
Dye, reduces methyl tin heat stabilizer and PVC product cost, wide market.
Enterprise uses heat-stable time and tenor to characterize the performance of methyl stannum antimony liquid composite thermal stabilizer product,
Wherein, antimony content be determined as an important part, the assay method of current antimony content mainly has potassium bromate method, iodimetric titration and instrument
Device analytic process etc., wherein when antimony content is bigger, instrumental method accuracy can be decreased obviously, and equipment price is expensive.Cause
This, potassium bromate method and iodimetric titration are the most conventional.
Chinese patent CN103969396B describes " detection method of antimony content in a kind of liquid form product ", and this invention includes
The dissolving preparation of liquid sample and calibrating two parts, the main content using potassium bromate method calibrating antimony, there is sample treatment
Complexity, response speed is relatively slow, and shortcoming is asked in titration end-point difficulty or ease judgement etc..
Report in " application chemical industry " volume 31 the 2nd phase document " research of determination of antimony content in complexes by iodimetry " in 2002
Indicator, with hydrochloric acid and sodium potassium tartrate tetrahydrate sample dissolution, is made with starch in road, uses iodine standard solution direct titration to measure antimony and joins
Compound kind antimony content.And methyl stannum antimony composite thermal stabilizer belongs to macromolecule organic, hydrochloric acid and sodium potassium tartrate tetrahydrate and is difficult to dissolve
Methyl stannum antimony composite thermal stabilizer, therefore cannot realize the detection of antimony content in methyl stannum antimony composite thermal stabilizer.Therefore, at present
Still without being suitable for the detection method of (macromolecule organic) antimony content in mensuration methyl stannum antimony liquid composite stabilizing agent.
Summary of the invention
It is an object of the invention to solve the method inapplicable mensuration methyl stannum antimony composite thermal stabilizer of prior art not
Foot, it is provided that one is simple to operate, sample treatment convenient, response speed is suitable, the methyl stannum antimony that titration end-point the most reliably judges
The assay method of composite thermal stabilizer antimony content.
The technical solution adopted for the present invention to solve the technical problems is:
Indirect iodometric processes measures the method for antimony content in methyl stannum antimony composite thermal stabilizer, and described assay method includes following
Step:
(1) weigh a certain amount of methyl stannum antimony composite thermal stabilizer sample, be sequentially added into concentrated sulphuric acid, concentrated nitric acid and high chlorine
Acid, three kinds of sour volume ratios are 2～3:1:1, and sample quality is 1:35～55, g/ml with the ratio of mixed acid volume, heating
Dissolving, treat that it is cooled to room temperature and adds (1+9) hydrochloric acid solution constant volume, the volume of constant volume is V, shakes up, standby；
(2) pipetting volume is V0Step (1) prepare solution, add appropriate potassium iodide and starch indicator, utilization rubs
The sodium thiosulfate standard titration solution titration of your concentration 0.01mol/L, becomes colorless as titration end-point, record to solution blueness
Consume the volume V of sodium thiosulfate standard titration solution1, doing blank assay simultaneously and writing down volume is V2, calculate by formula 1, i.e.
Obtain the antimony content in sample；
Formula 1:
In formula: C is the concentration of sodium thiosulfate standard solution, mol/L；
V1For the volume of the sodium thiosulfate standard titration solution that titration antimony consumes, ml；
V2By the volume of the sodium thiosulfate standard titration solution that blank assay is consumed, ml；
V is the volume of sample constant volume, ml；
V0For pipetting the volume of sample solution, ml after constant volume；
0.01218 is the quality of the antimony in grams suitable with 1.00ml sodium thiosulfate standard titration solution；
M is the quality of sample, g.
Methyl stannum antimony composite thermal stabilizer belongs to macromolecule organic, uses the method for routine to be difficult to make it dissolve, this
It is cleared up by the bright concentrated sulphuric acid using routine and concentrated nitric acid, but can not be complete, adds appropriate perchloric acid and coordinates by a certain percentage
Concentrated sulphuric acid and nitric acid use, and make sample accomplish thoroughly and clear up.The acid Acid system of the present invention selects rationally, selects so acid
Property environment, on the one hand tin ion is as easy as rolling off a log in this acid solution is hydrolyzed into stable tin compound, will not to the detection of antimony
Interference；On the other hand can fully and completely clear up sample, sample pretreatment is reliable, and subsequent measurements accuracy is high.
Preferably, in step (1), the volume ratio of concentrated sulphuric acid, concentrated nitric acid and perchloric acid is 2.5:1:1, and sample quality is with mixed
The ratio closing acid volume is 1:45, g/ml.
The invention has the beneficial effects as follows: the present invention solves the mensuration of methyl stannum antimony composite thermal stabilizer antimony content, result
Accurately, reliably, detecting instrument is simple simultaneously, and cost is relatively low, it is easy to promotion and application, exists for methyl stannum antimony composite thermal stabilizer
Application in PVC provides scientific basis.
Detailed description of the invention
Below in conjunction with specific embodiment, detection method of the present invention is described further, but in the protection of the present invention
Hold and be not limited to this.
One, main agents and instrument:
(1) sulphuric acid (concentration is 98%)
(2) nitric acid (concentration 68%)
(3) perchloric acid (concentration 70%)
(4) potassium iodide (content 99%)
(5) (1+9) hydrochloric acid solution: the mass ratio of hydrochloric acid and water is 1:9, concentration of hydrochloric acid is 37%.
(6) starch indicator (10g/l): weigh 1g starch and be placed in 250ml beaker, adds 100g water, is heated to starch
It is completely dissolved.
(7) sodium thiosulfate standard titration solution (0.01mol/L): accurately weigh 2.6000g sodium thiosulfate, 0.2g without
Aqueous sodium carbonate is placed in 1000ml beaker, adds 1000ml water, slowly boils 10min, be settled to 1000ml, molten with potassium dichromate
Liquid is demarcated, and uses after two weeks.
(8) burette (25ml)
Embodiment 1
(1) weigh methyl stannum antimony composite thermal stabilizer sample 0.2003g, be sequentially added into 5ml98% sulphuric acid, 2ml68% nitre
Acid and 2ml70% perchloric acid, heating for dissolving, treat that it is cooled to room temperature addition (1+9) hydrochloric acid solution and is settled to 100ml, shake up, standby
With.
(2) pipette the solution that 25ml step (1) prepares, add 0.5000g potassium iodide and 1ml10g/l starch indicator, profit
Titrate with 0.0101M sodium thiosulfate standard titration solution, become colorless as titration end-point, record consumption to solution blueness
The volume of sodium thiosulfate standard titration solution is V1, doing blank assay simultaneously and writing down volume is 0.00ml.Based on formula 1 is carried out
Calculate, the results are shown in Table 1.
Table 1 antimony content measurement result
Embodiment 2
Taking same monomethyl stannum antimony composite thermal stabilizer sample, separately sampled by analyzing together personnel, replication 6 times, to examine
Examine precision, the results are shown in Table 2.
Table 2 precision testing result
By Tables 1 and 2 it can be seen that the result of this method detection methyl stannum antimony composite thermal stabilizer antimony content is repeated
Good, accuracy is high.
In sum, the present invention can be advantageously used in the detection of methyl stannum antimony composite thermal stabilizer antimony content, and testing result is accurate
Really, reliably, without the need for expensive dedicated analysis instrument, cost is relatively low, it is easy to promotion and application, for methyl stannum antimony compound thermal
Stabilizer application in PVC provides scientific basis.
Embodiment described above is the one preferably scheme of the present invention, not makees the present invention any pro forma
Limit, on the premise of without departing from the technical scheme described in claim, also have other variant and remodeling.
Claims (2)
1. the method for antimony content during indirect iodometric processes measures methyl stannum antimony composite thermal stabilizer, it is characterised in that described mensuration side
Method comprises the following steps:
(1) weigh a certain amount of methyl stannum antimony composite thermal stabilizer sample, be sequentially added into mass fraction 95-98% concentrated sulphuric acid,
The concentrated nitric acid of mass fraction 65-68% and the perchloric acid of mass fraction 70-72%, three kinds of sour volume ratios are 2～3:1:1,
Sample quality is 1:35～55, g/ml with the ratio of mixed acid volume, heating for dissolving, treats that it is cooled to room temperature and adds (1+9) salt
Acid solution constant volume, the volume of constant volume is V, shakes up, standby；
(2) pipetting volume is V0Step (1) prepare solution, add appropriate potassium iodide and starch indicator, utilize molar concentration
The sodium thiosulfate standard titration solution titration of 0.01mol/L, becomes colorless as titration end-point, record consumption sulfur to solution blueness
The volume V of sodium thiosulfate standard titration solution1, doing blank assay simultaneously and writing down volume is V2, calculate by formula 1, obtain sample
In antimony content；
Formula 1:
In formula: C is the concentration of sodium thiosulfate standard solution, mol/L；
V1For the volume of the sodium thiosulfate standard titration solution that titration antimony consumes, ml；
V2By the volume of the sodium thiosulfate standard titration solution that blank assay is consumed, ml；
V is the volume of sample constant volume, ml；
V0For pipetting the volume of sample solution, ml after constant volume；
0.01218 is the quality of the antimony in grams suitable with 1.00ml sodium thiosulfate standard titration solution；
M is the quality of sample, g.
Indirect iodometric processes the most according to claim 1 measures the method for antimony content in methyl stannum antimony composite thermal stabilizer, its
Being characterised by: in step (1), the volume ratio of concentrated sulphuric acid, concentrated nitric acid and perchloric acid is 2.5:1:1, sample quality and mixed acid body
Long-pending ratio is 1:45, g/ml.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110836947A (en) * | 2018-08-15 | 2020-02-25 | 青岛海湾精细化工有限公司 | Method for detecting active ingredients of pyrazolone |
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| CN101921405A (en) * | 2010-08-17 | 2010-12-22 | 浙江海普顿化工科技有限公司 | Methyltin composite heat stabilizer and preparation method thereof |
| CN103969396A (en) * | 2014-05-14 | 2014-08-06 | 金浦新材料股份有限公司 | Method for detecting content of antimony in liquid product |
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- 2016-06-17 CN CN201610445414.4A patent/CN106124690A/en active Pending
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| US20100280155A1 (en) * | 2005-05-05 | 2010-11-04 | Galata Chemicals, Llc | Alkyltin Sulfanyl Mercaptocarboxylates Having Terminal Thiol Groups |
| CN101876654A (en) * | 2009-04-30 | 2010-11-03 | 山东松本电源科技有限公司 | Method for determining stibium in aluminum base alloy |
| CN101921405A (en) * | 2010-08-17 | 2010-12-22 | 浙江海普顿化工科技有限公司 | Methyltin composite heat stabilizer and preparation method thereof |
| CN103969396A (en) * | 2014-05-14 | 2014-08-06 | 金浦新材料股份有限公司 | Method for detecting content of antimony in liquid product |
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Application publication date: 20161116 |