CN101329226B - Method for preparing heavy metal ingredient standard substance in polyvinyl chloride - Google Patents
Method for preparing heavy metal ingredient standard substance in polyvinyl chloride Download PDFInfo
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- CN101329226B CN101329226B CN 200710047544 CN200710047544A CN101329226B CN 101329226 B CN101329226 B CN 101329226B CN 200710047544 CN200710047544 CN 200710047544 CN 200710047544 A CN200710047544 A CN 200710047544A CN 101329226 B CN101329226 B CN 101329226B
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Abstract
The invention relates to a preparation method used for researching and detecting the heavy metal composition standard substance in polyvinyl chloride (PVC) of electronic products, comprising the steps as follows: a: 0.4-4/1000 (parts by weight) of solid heavy metal is added into more than 1 (number part) of PVC master batch (with the parts by weight 1); b: the PVC and the solid heavy metal are respectively mixed uniformly; c: liquid heavy metal which is formed by the mixing of 0.2-2/1000 (parts by weight) of the heavy metal and 0.8-4mL (volume) of diluted solution are respectively added; d: the heavy metal and the diluent are respectively mixed uniformly; e: each part of the PVC master batches which contain the solid heavy metal and the liquid heavy metal are mixed uniformly; f: heating and melting are carried out so as to lead the solid heavy metal and the liquid heavy metal to be uniformly dispersed into the PVC master batches; g: plastic extruding forming is carried out in a plastic extruding machine; and h: required grains are prepared in a granulator. The preparation method of the invention provides magnitude tracing matters for daily detection for electronic plastic products, solves the problem that the detection data can be different due to factors such as different substrates, concentration gradient, and physical appearance, etc., and exactly ensures the monitoring on concentration of the heavy metal element of the electronic plastic products.
Description
Technical field
The present invention relates to metrology and measurement standard transmission of quantity value technical field, especially relate to the preparation method of heavy metal ingredient standard substance (standard model) in the Polyvinylchloride that is widely used in studying and monitor in the electric equipment products.
Background technology
European Union has announced WEEE instruction and ROHS instruction in 2003, substance is from July 1st, 2006, ban use of or limit the electronic electric equipment product that uses leaded (Pb), mercury (Hg), cadmium (Cd), sexavalent chrome objectionable impuritiess such as (Cr6+), China is on the rise in the foreign trade restriction in this field.How to successfully manage this instruction and become the serious problem of paying close attention to of producer that China produces electric equipment products.Plastics kind is various, 18 big resinoids are arranged, about more than 200 kind, tygon (PE), Polyvinylchloride (PVC), polypropylene (PP) etc. is still its main product, and about using the heavy metal restricted problem of plastics in the electronic and electrical equipment, at present both at home and abroad the standard substance relevant with heavy metal in the plastics has only the release of standard reference materials office of the European Community--the granular polyethylene standard specimen of----3.0*1.5mm that is the standard reference materials of matrix with the vinyon, this standard substance and we need the bigger matrix difference of Polyvinylchloride (PVC) plastics existence in the emphasis detected electrons electrical equipment, as adopt fluorescence method to detect, because the difference of matrix can cause 5～10 times of data differences, and concentration gradient, pattern in kind etc. also is difficult to satisfy the requirement of ROHS actual detected.China in the process of actual detected plastics content of beary metal, employed standard substance all be heavy metal in the water base body as standard substance because the otherness of matrix effect, measuring error can reach 5～10 times.
Summary of the invention
Technical matters to be solved by this invention provides the preparation method of heavy metal ingredient standard substance in a kind of Polyvinylchloride (standard model).The technical scheme that the present invention solves its technical matters employing is, the preparation method of heavy metal ingredient standard substance in the Polyvinylchloride, it comprises the steps: a, adds parts by weight respectively in the parts by weight of quantity umber more than 1 part are 1 polyvinyl chloride master batch is 0.4～4/1000 solid-state heavy metal; B, evenly stirring respectively; C, to add by parts by weight respectively be the liquid heavy metal that dilution that 0.2～2/1000 heavy metal and volume are 0.8～4mL mixes; D, stir respectively; E, each part polyvinyl chloride master batch that will all contain solid-state heavy metal, liquid heavy metal mix stirring; F, heating and melting make solid-state heavy metal, liquid heavy metal be distributed in the polyvinyl chloride master batch full and uniformly; G, extrusion molding shaping in extruding machine; H, in granulator, granulate.Technical matters to be solved by this invention also can further be solved by following technical solution: i, pulverize in comminutor; J, heating and melting make solid-state heavy metal, liquid heavy metal be distributed in the polyvinyl chloride master batch full and uniformly; K, extrusion molding shaping in extruding machine; L, in granulator, granulate; The quantity umber is 25 parts more than 1 part; Solid-state heavy metal is that potpourri, its ratio of weight and number of dibasic lead stearate and potassium dichromate is 1/3; Liquid heavy metal is the potpourri of heavy metal and dilution, and heavy metal is Cd sheet, Hg, and the ratio of weight and number of Cd sheet and Hg is 1/1 or 1/10, and dilution is 65～68% technology super-pure nitric acids; The temperature of heating and melting is 210 ℃～220 ℃; Extrusion molding is configured as strip.
The present invention can continue the following step: i, pulverize in comminutor after the granulation; J, heating and melting; K, extrusion molding shaping in extruding machine; L, in granulator, granulate, make solid-state heavy metal, liquid heavy metal be distributed in the polyvinyl chloride master batch full and uniformly, attain to better invention effect.Polyvinyl chloride master batch among the present invention, Cd sheet, Hg, dibasic lead stearate, potassium dichromate, 65～68% technology super-pure nitric acids all can be buied from the chemical reagent shop.Prepare stirring machine of the present invention, extruding machine, granulator, comminutor and heating and melting equipment and be the commercially available universal product.The present invention provides the magnitude tracing material for daily electronic apparatus plastic product detects; solved matrix difference; concentration gradient; factors such as pattern in kind can cause detecting the data difference problem; accurately guaranteed monitoring to the heavy metal element concentration in the electronic apparatus plastic product; not only protected the environment and the people's health; and China's Related product is squeezed into the international market; the technology barriers of breaking in the international trade have been cleared away obstacle; for the import and export of national electric equipment products provide the reliable detection standard substance; guaranteed the technology status in the interests in international trade and China commodity inspection work after the China joined WTO; social benefit has a far reaching influence, and has also remedied the blank spot in heavy metal ingredient standard substance field in Polyvinylchloride simultaneously.
Embodiment
Embodiment 1: get 25 parts, every part 1Kg of polyvinyl chloride master batch; Add solid-state heavy metal dibasic lead stearate 0.1g and potassium dichromate 0.3g and evenly stir at each part polyvinyl chloride master batch with stirring machine; in each part polyvinyl chloride master batch, add the liquid heavy metal that mixes by heavy metal and dilution; heavy metal in the liquid heavy metal is the Cd sheet; Hg; the ratio of weight and number of Cd sheet and Hg is 1/1; dilution is 65～68% technology super-pure nitric acids; get Cd sheet 0.1g; Hg0.1g also uses 0.8mL65～68% technology super-pure nitric acid dissolving; again 25 parts of polyvinyl chloride master batch are mixed stirring after respectively 25 parts of polyvinyl chloride master batch (having contained solid-state heavy metal and liquid heavy metal) being stirred; at 210 ℃～220 ℃; preferably under 215 ℃ the temperature to the polyvinyl chloride master batch heating and melting; make solid-state heavy metal; liquid heavy metal is distributed in the polyvinyl chloride master batch full and uniformly; with commercially available extruding machine polyvinyl chloride master batch is extruded into strip; in granulator, granulate, can realize goal of the invention of the present invention.
Embodiment 2: get 25 parts, every part 1Kg of polyvinyl chloride master batch; Add solid-state heavy metal dibasic lead stearate 1g and potassium dichromate 3g and evenly stir at each part polyvinyl chloride master batch with stirring machine; in each part polyvinyl chloride master batch, add the liquid heavy metal that mixes by heavy metal and dilution; heavy metal in the liquid heavy metal is the Cd sheet; Hg; the ratio of weight and number of Cd sheet and Hg is 1/10; dilution is 65～68% technology super-pure nitric acids; get Cd sheet 0.1g; Hg1g also uses 2.4mL65～68% technology super-pure nitric acid dissolving; again 25 parts of polyvinyl chloride master batch are mixed stirring after respectively 25 parts of polyvinyl chloride master batch (having contained solid-state heavy metal and liquid heavy metal) being stirred; at 210 ℃～220 ℃; preferably under 215 ℃ the temperature to the polyvinyl chloride master batch heating and melting; make solid-state heavy metal; liquid heavy metal is distributed in the polyvinyl chloride master batch full and uniformly; with commercially available extruding machine polyvinyl chloride master batch is extruded into strip; in granulator, granulate, can realize goal of the invention of the present invention.
Embodiment 3: get 25 parts, every part 1Kg of polyvinyl chloride master batch; Add solid-state heavy metal dibasic lead stearate 1g and potassium dichromate 3g and evenly stir at each part polyvinyl chloride master batch with stirring machine; in each part polyvinyl chloride master batch, add the liquid heavy metal that mixes by heavy metal and dilution; heavy metal in the liquid heavy metal is the Cd sheet; Hg; the ratio of weight and number of Cd sheet and Hg is 1/1; dilution is 65～68% technology super-pure nitric acids; get Cd sheet 1g; Hg1g also uses 4mL65～68% technology super-pure nitric acid dissolving; again 25 parts of polyvinyl chloride master batch are mixed stirring after respectively 25 parts of polyvinyl chloride master batch (having contained solid-state heavy metal and liquid heavy metal) being stirred; at 210 ℃～220 ℃; preferably under 215 ℃ the temperature to the polyvinyl chloride master batch heating and melting; make solid-state heavy metal; liquid heavy metal is distributed in the polyvinyl chloride master batch full and uniformly; with commercially available extruding machine polyvinyl chloride master batch is extruded into strip; in granulator, granulate, can realize goal of the invention of the present invention.
The above embodiment of the present invention all can continue the following step: i, pulverize in comminutor after the granulation; J, heating and melting; K, extrusion molding shaping in extruding machine; L, in granulator, granulate, make solid-state heavy metal, liquid heavy metal be distributed in the polyvinyl chloride master batch full and uniformly, attain to better invention effect.
The present invention has made the quantification of determining with the heavy metal in the Polyvinylchloride, the standard substance (standard model) that whether exceeds standard as the heavy metal that detects in the Polyvinylchloride.The present invention through Science and Technology of Shanghai Cha Xin referral centre of the Chinese Academy of Sciences look into new and project to seek advice from conclusion as follows: " this project has novelty and novelty, and having filled up China's plastics is the blank of the heavy metal standard substance of matrix ".
The present invention develops complex art and is in a leading position at home, and has reached international most advanced level.
Claims (7)
1. the preparation method of heavy metal ingredient standard substance in the Polyvinylchloride is characterized in that it comprises the steps:
A, to add parts by weight respectively in the parts by weight of quantity umber more than 1 part are 1 polyvinyl chloride master batch be 0.4～4/1000 solid-state heavy metal;
B, evenly stirring respectively;
C, to add by parts by weight respectively be the liquid heavy metal that dilution that 0.2～2/1000 heavy metal and volume are 0.8～4mL mixes;
D, stir respectively;
E, each part polyvinyl chloride master batch that will all contain solid-state heavy metal, liquid heavy metal mix stirring;
F, heating and melting make solid-state heavy metal, liquid heavy metal be distributed in the polyvinyl chloride master batch full and uniformly;
G, extrusion molding shaping in extruding machine;
H, in granulator, granulate.
2. the preparation method of heavy metal ingredient standard substance in the Polyvinylchloride according to claim 1 is characterized in that it also comprises the steps:
I, in comminutor, pulverize;
J, heating and melting make solid-state heavy metal, liquid heavy metal be distributed in the polyvinyl chloride master batch full and uniformly;
K, extrusion molding shaping in extruding machine;
L, in granulator, granulate.
3. the preparation method of heavy metal ingredient standard substance in the Polyvinylchloride according to claim 1 and 2 is characterized in that: the quantity umber is 25 parts more than 1 part.
4. the preparation method of heavy metal ingredient standard substance in the Polyvinylchloride according to claim 1 and 2 is characterized in that: solid-state heavy metal is that potpourri, its ratio of weight and number of dibasic lead stearate and potassium dichromate is 1/3.
5. the preparation method of heavy metal ingredient standard substance in the Polyvinylchloride according to claim 1 and 2, it is characterized in that: liquid heavy metal is the potpourri of heavy metal and dilution, heavy metal is Cd sheet, Hg, the ratio of weight and number of Cd sheet and Hg is 1/1 or 1/10, and dilution is 65～68% technology super-pure nitric acids.
6. the preparation method of heavy metal ingredient standard substance in the Polyvinylchloride according to claim 1 and 2 is characterized in that: the temperature of heating and melting is 210 ℃～220 ℃.
7. the preparation method of heavy metal ingredient standard substance in the Polyvinylchloride according to claim 1 and 2, it is characterized in that: extrusion molding is configured as strip.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710047544 CN101329226B (en) | 2007-10-29 | 2007-10-29 | Method for preparing heavy metal ingredient standard substance in polyvinyl chloride |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200710047544 CN101329226B (en) | 2007-10-29 | 2007-10-29 | Method for preparing heavy metal ingredient standard substance in polyvinyl chloride |
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| CN101329226A CN101329226A (en) | 2008-12-24 |
| CN101329226B true CN101329226B (en) | 2010-09-08 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103308358B (en) * | 2013-04-20 | 2016-05-04 | 东莞龙昌智能技术研究院 | The preparation method of the Analysis of Heavy Metal standard substance of a kind of modified polyvinyl chloride and ABS mixture |
| CN103604678A (en) * | 2013-12-09 | 2014-02-26 | 广州赛宝计量检测中心服务有限公司 | Sample preparation method for uniformly distributing trace components in solid block matrix |
| CN106769274B (en) * | 2016-11-09 | 2019-06-21 | 金发科技股份有限公司 | A kind of preparation method of the ABS standard sample for X-ray fluorescence spectra analysis |
| CN107917908A (en) * | 2017-03-07 | 2018-04-17 | 蒋小良 | A kind of dermatine heavy metal standard substance and preparation method |
| JP6366767B1 (en) * | 2017-03-24 | 2018-08-01 | 株式会社日立ハイテクサイエンス | Manufacturing method of plastic reference materials |
| CN111413170B (en) * | 2020-04-16 | 2020-10-09 | 南京市计量监督检测院 | Preparation method of heavy metal standard substance of crayfish matrix |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001052527A (en) * | 1999-08-05 | 2001-02-23 | Fujikura Ltd | Non-halogen flame retardant resin composition and molding product using it |
| CN1715872A (en) * | 2004-06-28 | 2006-01-04 | 富士康(昆山)电脑接插件有限公司 | Continuous detecting method for lead-cadmium in plastic sample |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001052527A (en) * | 1999-08-05 | 2001-02-23 | Fujikura Ltd | Non-halogen flame retardant resin composition and molding product using it |
| CN1715872A (en) * | 2004-06-28 | 2006-01-04 | 富士康(昆山)电脑接插件有限公司 | Continuous detecting method for lead-cadmium in plastic sample |
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