CN103396702B - Preparation method of heavy metal-containing crayon standard sample for laboratory capability verification - Google Patents
Preparation method of heavy metal-containing crayon standard sample for laboratory capability verification Download PDFInfo
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- CN103396702B CN103396702B CN201310360505.4A CN201310360505A CN103396702B CN 103396702 B CN103396702 B CN 103396702B CN 201310360505 A CN201310360505 A CN 201310360505A CN 103396702 B CN103396702 B CN 103396702B
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Abstract
The present invention discloses a heavy metal-containing crayon standard sample for laboratory capability verification, a preparation method and applications thereof. According to the heavy metal-containing crayon standard sample for laboratory capability verification, relative deviation of detection results does not exceed 15%, standard deviation of sample nonuniformity is not more than 0.3sigma, sample uniformity and stability meet capability verification sample requirements, the blank that the class of the capability verification samples do not exists in our country is filled, and a detection level of a laboratory participating in capability verification is increased.
Description
Technical field:
The present invention relates to a kind of preparation method of the wax crayon standard model that contains heavy metal that is applied to laboratory proficiency testing.
Background technology:
At present, along with the pay attention to day by day of international community to consumer's goods safety, in the consumer's goods such as toy, the detection of harmful chemical is increasing, except traditional heavy metal, softening agent, azo, dihydroxyphenyl propane, organo-tin compound etc. all strictly limited, correspondingly, consumer's goods chemical detection project and testing laboratory are on the increase, taking toy product detection as example, chemical detection workload accounts for all events and detects proportion up to 80%, obtains nearly 200 of CNAS accreditation toy specialty testing laboratory; Meanwhile, proficiency testing seems and becomes more and more important for quality control and the Laboratory Accreditation management etc. in laboratory self, and related request constantly adds sternly.CNAS issues new edition RL02 " proficiency testing rule " in February, 2011, wherein 4.2.3 is revised as by " application accreditation ... at least participate in a proficiency testing plan " that " each sub-field of conformity assessment body application accreditation should at least be participated in an ability verification and be obtained satisfactory result.", the technical requirements of this clause when adding tight conformity assessment body application accreditation; Toy inspection field is also added in CNAS-AL07 " CNAS proficiency testing field and frequency table " file, the chemical analyses such as toy has clearly been proposed to the requirement of 1 times/year.
Wax crayon is widely used by children as drawing, writing implement, the objectionable impurities harm children's that children's wax crayon may contain health, the restriction of children's wax crayon is equal to toy both at home and abroad, also the transportable heavy metal content of children's wax crayon is had to strict restriction at China GB6675-2003 toys standard.In addition, the safety general of GB21027-2007 students' supplies has also been made the regulation consistent with GB6675 to transportable heavy metal content in requiring.Estimate, obtain accordingly accredited laboratory and surpass 100.The transportable Heavy metal of GB6675-2003 comprises various dissimilar materials, the transportable Heavy metal proficiency testing of the toy plan that CNAS carried out is in the past mainly at paint coating material, the materials such as shorter mention wax crayon, and because the detection method of differing materials has very big-difference in sample pre-treatments, in wax crayon, transportable heavy metal content test is more complicated than paint aspect sample pre-treatments, before extraction, increase paraffin removal step, extraction step is also different, and the uncertain factor of its detected result is increased.
In addition, due to wax crayon be generally at high temperature paraffin melt into wax liquid then coagulation forming become solid, and toner cannot be dissolved in wax liquid, paraffin is difficult to be mixed with heavy metal toner, thereby is difficult to obtain all even stable wax crayon samples.
At present, in the actual wax crayon sample that contains heavy metal detecting, the wax crayon that contains heavy metal sample that detect or that detected result is positive is considerably less, and the homogeneity of these samples is difficult to meet the requirement of proficiency testing.
In sum, be not still applied to wax crayon standard model that contains heavy metal of laboratory proficiency testing and preparation method thereof at present.Develop a kind of wax crayon standard model that contains heavy metal that is applied to laboratory proficiency testing to meet proficiency testing requirement, having filled up China does not have the blank of such proficiency testing sample at present, has improved the detection level of participating in proficiency testing laboratory simultaneously yet.
Summary of the invention:
The object of this invention is to provide a kind of preparation method of the wax crayon standard model that contains heavy metal that is applied to laboratory proficiency testing.
The present invention is achieved by the following technical programs:
A preparation method who is applied to the wax crayon standard model that contains heavy metal of laboratory proficiency testing, comprises the following steps:
A, add toward crossing in the talcum powder, pigment of 800 mesh sieves the compound powder that contains heavy metal element, and then add the vasoliniment having melted, then mixture is fully uniformly mixed until color even is consistent; Described heavy metal is lead, barium, cadmium and chromium; by final product mass percent; described talcous concentration is 9%; the concentration of pigment is 0.1～1%; in heavy metal, the concentration range of every kind of element is that 25-10000mg/kg(is in element quality), the concentration of the vasoliniment having melted that step a adds is 3%;
B, the material mixing is above positioned in plastic containers, is then put on three rod shredders and grinds, repeated several times to each component is uniformly dispersed, and is positioned in plastic containers for subsequent use after grinding;
In c, the material that obtains toward step b, continue to add the vasoliniment having melted, supply 100%, mix, be then put in stainless steel vessel, be constantly stirred to uniform state;
D, the material that step c is obtained pour in the mould of wax crayon machine, carry out cooling, coagulation forming;
E, the solid material after moulding is carried out to the demoulding, obtain the wax crayon standard model of the heavy metal that contains different concns.
The described compound powder that contains heavy metal element is preferably Pb
3o
4or PbCrO4, BaB
2o
4, CdS, K
2cr
2o
4or/PbCrO4.Preferred concentration range is 250-1300mg/kg.
The wax crayon standard model of the heavy metal that contains different concns prepared in accordance with the present invention, for the proficiency testing of laboratory wax crayon class testing project, for detection of the checking of method.
The present invention obtain the wax crayon standard model that contains heavy metal that is applied to laboratory proficiency testing, detected result relative deviation is no more than 15%, sample ununiformity standard deviation is not more than 0.3 σ, the homogeneity of sample and stability meet the requirement of proficiency testing sample, fill up the blank that China does not have such proficiency testing sample at present, improved the detection level of participating in proficiency testing laboratory.
Embodiment:
Below to further illustrate of the present invention, instead of limitation of the present invention.
Taking the formula of 3 kilograms of total masses as example, the preparation method that the present invention is applied to the wax crayon standard model that contains heavy metal of laboratory proficiency testing comprises the following steps:
A, in the talcum powder of 0.27 kilogram of mistake 800 mesh sieve, 3 grams of pigment, add 2.5 grams of BaB
2o
4, 1.8 grams of CdS, 4.9 grams of PbCrO
4, 0.68 gram of Pb
3o
4heavy metal powder, for avoiding heavy metal caking to cause mixing inequality, first grinds to form heavy metal heavy metal powder, and then adds the 0.09 kilogram of vasoliniment 1 having melted, then mixture is fully uniformly mixed until color even is consistent; Barium, cadmium, lead, the concentration of chromium element is respectively 513mg/kg, 467mg/kg, 1253mg/kg, this concentration range of 263mg/kg(be 25-10000mg/kg all can);
B, the material mixing is above positioned in plastic tub, is then put on three rod shredders and grinds, each grinding got 200 grams, repeat 10 times, object is to make heavy metal powder, talcum powder, the paraffin of pigment and melting is uniformly dispersed together with evenly grinding, and is positioned in plastic tub for subsequent use after grinding;
In c, the material that obtains toward step b, continue to add the vasoliniment having melted until product total mass is 3 kilograms, mix, be then put in stainless steel pot, be constantly stirred to uniform state;
D, the material that step c is obtained pour in the mould of wax crayon machine, carry out cooling, coagulation forming;
E, the solid material after moulding is carried out to the demoulding, obtain the wax crayon standard model of the heavy metal that contains different concns.
The wax crayon standard model that embodiment 1 is obtained is got at random 10 samples and is carried out homogeneity detection, twice of each sample replicate measurement, (concentration of moving out adopts GB6675-2003 appendix C .8.7 to detect to obtain concentration that lead, barium, cadmium, chromium four heavy metal species moves out, the final concentration of moving out of described heavy metal is to use 1,1,1-trichloroethane or other suitable solvents are extracted wax composition are removed by dissolving.Then with being equivalent to 50 times of wax crayon sample qualities, temperature is that the hydrochloric acid soln that the concentration of 37 ± 2 DEG C is 0.07mol/L moves out of the concentration of lead, barium, cadmium, chromium four heavy metal species, so the four heavy metal species results of moving out will be lower than the heavy metal concentration adding) detected result is as shown in table 1.
The single factor two level detection results of table 1
According to ISO13528:2005(E) appendix C algorithm A carries out analytical calculation, and result is as shown in table 2.
Table 2 sample homogeneity test the results of analysis of variance
The F0.05 (9,10)=3.02 that tables look-up, statistic F value is all less than threshold value, and result shows: sample room there was no significant difference, the proficiency testing article that draw preparation are uniform.
This proficiency testing is proficiency testing article ununiformity standard deviation S s≤0.3 σ in the works, further verified this proficiency testing in the works proficiency testing article be uniform.
Standard wax crayon sample has been used to organizational capacity checking activity, assign to 61 laboratories by detecting qualified sample through homogeneity, carry out according to unified experimental arrangement the concentration that lead, barium, cadmium, chromium four heavy metal species moves out and detect, detected result and statistics table are as shown in table 3.
Table 3 laboratory detection result and statistics table
Note: # represents it is problem result; § meaning result with thumb down.
The present invention obtain the wax crayon standard model that contains heavy metal that is applied to laboratory proficiency testing, detected result relative deviation is no more than 15%, sample ununiformity standard deviation is not more than 0.3 σ, and the homogeneity of sample and stability meet the requirement of proficiency testing sample.
Claims (2)
1. a preparation method who is applied to the wax crayon standard model that contains heavy metal of laboratory proficiency testing, comprises the following steps:
A, add toward crossing in the talcum powder, pigment of 800 mesh sieves the compound powder that contains heavy metal element, described in contain heavy metal element compound powder be selected from following compound: Pb
3o
4or PbCrO4, BaB
2o
4, CdS, K
2cr
2o
4or PbCrO4, and then add the vasoliniment having melted, then mixture is fully uniformly mixed until color even is consistent; Described heavy metal is lead, barium, cadmium and chromium, by final product mass percent, described talcous concentration is 9%, and the concentration of pigment is 0.1～1%, in heavy metal, the concentration range of every kind of element is 25-10000mg/kg, and the concentration of the vasoliniment having melted that step a adds is 3%;
B, the material mixing is above positioned in plastic containers, is then put on three rod shredders and grinds, repeated several times to each component is uniformly dispersed, and is positioned in plastic containers for subsequent use after grinding;
In c, the material that obtains toward step b, continue to add the vasoliniment having melted and supply 100%, mix, be then put in stainless steel vessel, be constantly stirred to uniform state;
D, the material that step c is obtained pour in the mould of wax crayon machine, carry out cooling, coagulation forming;
E, the solid material after moulding is carried out to the demoulding, obtain the wax crayon standard model of the heavy metal that contains different concns.
2. the preparation method of the wax crayon standard model that contains heavy metal that is applied to laboratory proficiency testing according to claim 1, is characterized in that, in described heavy metal, the concentration range of every kind of element is 250-1300mg/kg.
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| CN103396702B true CN103396702B (en) | 2014-09-03 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103728170B (en) * | 2014-01-07 | 2015-10-28 | 中华人民共和国北京出入境检验检疫局 | Proficiency testing sample of and chrome determination plumbous for textile extractable heavy metal and preparation method thereof |
| CN106496786A (en) * | 2016-10-25 | 2017-03-15 | 浙江省家具与五金研究所 | Heavy metal standard sample and preparation method thereof in a kind of PP wood mouldings |
| CN106751217B (en) * | 2016-12-28 | 2018-10-26 | 广东出入境检验检疫局检验检疫技术中心 | A kind of preparation method of plasticizer-containing plastic cement standard sample |
| CN108132169B (en) * | 2017-12-07 | 2020-04-21 | 中国航发动力股份有限公司 | Method for manufacturing laboratory capacity comparison sample |
| CN110079149B (en) * | 2019-05-28 | 2022-02-11 | 福建中烟工业有限责任公司 | Printing ink, standard substance, preparation method and application thereof |
| CN111323282B (en) * | 2020-04-10 | 2022-09-06 | 广州海关技术中心 | Preparation method of paint powder standard sample containing 17 migratable elements limited in toy field |
| CN113776902A (en) * | 2021-08-16 | 2021-12-10 | 拱北海关技术中心 | Preparation method of reference standard substance for detecting impurities in aluminum pigment |
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|---|---|---|---|---|
| CN1053627A (en) * | 1989-12-19 | 1991-08-07 | 联合碳化化学品及塑料有限公司 | Water soluble crayon composition |
| CN101033354A (en) * | 2007-04-10 | 2007-09-12 | 上海乐美文具有限公司 | Water-based multipurpose painting pen |
| CN101511953A (en) * | 2006-09-04 | 2009-08-19 | 樱花彩色产品株式会社 | Crayon and method for producing the same |
| CN101993636A (en) * | 2009-08-17 | 2011-03-30 | 真彩文具有限公司 | Crayon and manufacturing method thereof |
| CN102533005A (en) * | 2010-12-30 | 2012-07-04 | 刘颖 | Colorful high-elastoplastic pen and making method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0433970A (en) * | 1990-05-29 | 1992-02-05 | Pentel Kk | Solid painting material |
-
2013
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1053627A (en) * | 1989-12-19 | 1991-08-07 | 联合碳化化学品及塑料有限公司 | Water soluble crayon composition |
| CN101511953A (en) * | 2006-09-04 | 2009-08-19 | 樱花彩色产品株式会社 | Crayon and method for producing the same |
| CN101033354A (en) * | 2007-04-10 | 2007-09-12 | 上海乐美文具有限公司 | Water-based multipurpose painting pen |
| CN101993636A (en) * | 2009-08-17 | 2011-03-30 | 真彩文具有限公司 | Crayon and manufacturing method thereof |
| CN102533005A (en) * | 2010-12-30 | 2012-07-04 | 刘颖 | Colorful high-elastoplastic pen and making method thereof |
Non-Patent Citations (1)
| Title |
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| JP平4-33970A 1992.02.05 |
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