CN103471880A - Nickel release detection standard substance preparation method - Google Patents
Nickel release detection standard substance preparation method Download PDFInfo
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- CN103471880A CN103471880A CN2013103435814A CN201310343581A CN103471880A CN 103471880 A CN103471880 A CN 103471880A CN 2013103435814 A CN2013103435814 A CN 2013103435814A CN 201310343581 A CN201310343581 A CN 201310343581A CN 103471880 A CN103471880 A CN 103471880A
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Abstract
The present invention relates to a nickel release detection standard substance preparation method, which comprises: uniformly mixing brass powder and nickel powder according to a certain ratio to prepare a pre-smelting raw material; placing the raw material in a graphite crucible, adding a layer of active carbon powder on the surface, and placing into an intermediate frequency induction device; setting an initial induction current to 70+/-5 A, carrying out heat smelting, and maintaining for 3-5 min; reducing the current value to 50+/-5 A, and maintaining for 1-2 min; repeatedly performing the previous steps three times, and carrying out argon gas protection during the processes; increasing the current value to 80 A, heating for 0.5-1 min, and then pouring into a graphite mold to prepare a round bar-like specimen; cutting the specimen into a sheet with phi20*1.3 mm, grinding to achieve a thickness of 1.2 mm and a weight of about 3.0 g; and cleaning the grinded specimen with alcohol, and carrying out hot air drying. The preparation method has characteristics of simple process, strong production operability, easy operation, low cost, easily available raw materials, and easy marketization, wherein the obtained standard substance has good uniformity and good stability.
Description
Technical field
The present invention relates to a kind of preparation method of nickel burst size examination criteria product.
Background technology
Nickel is widely used in manufactures jewellery, coin, Metal buttons etc., and nickel is the modal reason that causes contact allergy, approximately has 10% ~ 20% women can produce allergy to nickel.The nickel ion that the long-term absorption of skin discharges from the nickel-containing material of direct and skin contact, produce allergy, further is exposed in soluble nickel salt and can generation anaphylaxis contacts dermatitis.European Parliament and the instruction 94/27/EC(OJ No.L188 of 22.7.94 of EU Council) the rate of release threshold value of regulation nickel is 0.5 μ g/cm
2week.
At present domestic have many third parties testing agency in the test of carrying out the nickel burst size, but the domestic standard items that still detect without the nickel burst size at present, the standard items that nickel burst size at present commonly used detects are generally from external import, to mix and make with gold and nickel, cost is higher, and its homogeneity and stability await further raising.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method of nickel burst size examination criteria product, the method technique is simple, produce workable, simple operation; The standard items cost of producing with this method is low, and material is easy to get, the more easily marketization, and homogeneity and good stability.
The present invention is achieved by the following technical solutions, and a kind of preparation method of nickel burst size examination criteria product comprises following three steps:
(1) preparation of raw material: brass powder is evenly mixed in certain proportion with nickel powder, be mixed with the presmelting raw material;
(2) melting: a) the 1kg left and right presmelting raw material of step (1) gained is placed in graphite crucible, adds the layer of active carbon powder on presmelting raw material surface in case oxidation, then be positioned in Medium frequency induction equipment; B) setting initial induction current is 70 ± 5 A, adds hot smelting, in fusion process, with graphite rod, is stirred, and every 2 minutes, stirs once, continues about 3～5 minutes; C) turn down current value to 50 ± 5 A when evaporation is more violent, continue about 1～2 minute; D) step b, c are operated 3 times repeatedly, carry out argon shield in process; E) cast is heightened current value to 80 A before melt, heat 0.5～1 minute, and stirred with graphite rod, then rapidly by melt cast to graphite jig, make it the cooling pole shape of making;
(3) cutting polishing: the pole shape sample that a) will smelt and pour into a mould cuts into the sheet specimens of Φ 20 * 1.3 mm by the mode of spark cutting; B) with No. 400 adamas sand paper by specimen surface polish to thickness be 1.2mm, the heavily about 3.0g of sheet; C) sample of having polished is cleaned with alcohol, hot blast drying, obtain nickel burst size examination criteria product.
The mass ratio of brass powder of the present invention and nickel powder is 100:5 and 100:2.5, to make 5% A sample standard items and 2% B sample standard items.
The purity of brass powder of the present invention is: 80～95%.
The invention has the beneficial effects as follows: a kind of preparation method of nickel burst size examination criteria product, the method technique is simple, produce workable, simple operation; The standard items cost of producing with this method is low, and material is easy to get, the more easily marketization, and homogeneity and good stability.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
The preparation of 5% A sample standard items.
(1) preparation of raw material: brass powder is evenly mixed with the mass ratio of nickel powder with 100:5, be mixed with the presmelting raw material;
(2) melting: a) the 1kg left and right presmelting raw material of step (1) gained is placed in graphite crucible, adds the layer of active carbon powder on presmelting raw material surface in case oxidation, then be positioned in Medium frequency induction equipment; B) setting initial induction current is 75 A, adds hot smelting, in fusion process, with graphite rod, is stirred, and every 2 minutes, stirs once, continues about 3 minutes; C) turn down current value to 50 A when evaporation is more violent, continue about 2 minutes; D) step b, c are operated 3 times repeatedly, carry out argon shield in process; E) cast is heightened current value to 80 A before melt, heat 1 minute, and stirred with graphite rod, then rapidly by melt cast to graphite jig, make it the cooling pole shape of making;
(3) cutting polishing: the pole shape sample that a) will smelt and pour into a mould cuts into the sheet specimens of Φ 20 * 1.3 mm by the mode of spark cutting; B) with No. 400 adamas sand paper by specimen surface polish to thickness be 1.2mm, the heavily about 3.0g of sheet; C) sample of having polished is cleaned with alcohol, hot blast drying, obtain 5% A sample standard items.
Embodiment 2
The preparation of 2% B sample standard items.
(1) preparation of raw material: brass powder is evenly mixed with the mass ratio of nickel powder with 100:2.5, be mixed with the presmelting raw material;
(2) melting: a) the 1kg left and right presmelting raw material of step (1) gained is placed in graphite crucible, adds the layer of active carbon powder on presmelting raw material surface in case oxidation, then be positioned in Medium frequency induction equipment; B) setting initial induction current is 70 A, adds hot smelting, in fusion process, with graphite rod, is stirred, and every 2 minutes, stirs once, continues about 5 minutes; C) turn down current value to 52 A when evaporation is more violent, continue about 2 minutes; D) step b, c are operated 3 times repeatedly, carry out argon shield in process; E) cast is heightened current value to 80 A before melt, heat 0.5 minute, and stirred with graphite rod, then rapidly by melt cast to graphite jig, make it the cooling pole shape of making;
(3) cutting polishing: the pole shape sample that a) will smelt and pour into a mould cuts into the sheet specimens of Φ 20 * 1.3 mm by the mode of spark cutting; B) with No. 400 adamas sand paper by specimen surface polish to thickness be 1.2mm, the heavily about 3.0g of sheet; C) sample of having polished is cleaned with alcohol, hot blast drying, obtain 2% B sample standard items.
In order further to prove superiority of the present invention, the standard items that the present invention is produced have carried out the detection of homogeneity and stability, and homogeneity and stability are the important parameters of judgement nickel burst size examination criteria product quality, are determining the accuracy of nickel burst size test.
One, the uniformity testing of standard items
From packaged standard items, randomly draw 10 groups of samples for uniformity testing.For the every group of sample extracted, with random order, measure 2 times under the same conditions, adopt one-factor analysis of variance method to carry out statistical treatment to the result after checking.Assay (result of calculation is pressed EN1811:2011, testing result is not carried out to coefficient correction) is as shown in (table one).
Table one standard items homogeneity data summary table
As shown in Table 1, the F value that wherein the F value of A sample standard items is 1.15, B sample standard items is 1.56, by
fdistribution table checks in
f 0.05(9,10)=3.02, the F value of A sample standard items and B sample standard items all is less than
f 0.05(9,10), show in 95% fiducial interval, the nickel burst size there was no significant difference of sample room, the having good uniformity of sample.
For having good uniformity of standard items that further proof the present invention produces, following spy provides uniformity testing data from the nickel burst size examination criteria product of foreign procurement, and (result of calculation is pressed EN1811:2011, testing result is not carried out to coefficient correction), as shown in (table two).
The standard items homogeneity data summary table of table two foreign procurement
As can be seen from Table II, the standard items of foreign procurement have extracted equally 10 groups of samples and have tested, the F value of its uniformity testing is 2.61, and the F value of the A sample standard items that prepare by method of the present invention and B sample standard items is respectively 1.15 and 1.56, be less than the F value of the standard items of foreign procurement, the F value is larger, and sample is more inhomogeneous, this shows that the homogeneity of the standard items that prepare with the present invention is better than the standard items of foreign procurement.
Two, the stability test of standard items
Choose at random the A sample standard items of 6 part 5% for the check of stability, adopt
tmethod of inspection, the consistance between two mean values that obtain is measured in the comparative experiments chamber.Stability has been carried out 5 times and has been detected, and the time total span is 145 days, has contained 5 testing results of whole sense cycle, detects the result contrast in each test result and on June 8th, 2012 and carries out consistency checking, as shown in (table three).
Table three A sample standard items stability data statistic summary table
As shown above, the t value of A sample standard items stability test is respectively 1.232,0.242,0.341,1.76, all is less than t
0.05(10)=2.228 show that when 0.05 level of signifiance A sample standard items are stable in sense cycle.
By above check data, can be found out, the standard items homogeneity of utilizing the present invention to produce and having good stability, can fully meet the detection demand of nickel burst size, and cost is low, and production technology is simple, and easily preparation, can be promoted widely and apply.
Claims (3)
1. the preparation method of nickel burst size examination criteria product comprises following three steps:
(1) preparation of raw material: brass powder is evenly mixed in certain proportion with nickel powder, be mixed with the presmelting raw material;
(2) melting: a) the 1kg left and right presmelting raw material of step (1) gained is placed in graphite crucible, adds the layer of active carbon powder on presmelting raw material surface in case oxidation, then be positioned in Medium frequency induction equipment; B) setting initial induction current is 70 ± 5 A, adds hot smelting, in fusion process, with graphite rod, is stirred, and every 2 minutes, stirs once, continues about 3～5 minutes; C) turn down current value to 50 ± 5 A when evaporation is more violent, continue about 1～2 minute, d) step b, c are operated 3 times repeatedly, carry out argon shield in process; E) cast is heightened current value to 80 A before melt, heat 0.5～1 minute, and stirred with graphite rod, then rapidly by melt cast to graphite jig, make it the cooling pole shape of making;
(3) cutting polishing: the pole shape sample that a) will smelt and pour into a mould cuts into the sheet specimens of Φ 20 * 1.3 mm by the mode of spark cutting; B) with No. 400 adamas sand paper by specimen surface polish to thickness be 1.2mm, the heavily about 3.0g of sheet; C) sample of having polished is cleaned with alcohol, hot blast drying, obtain nickel burst size examination criteria product.
2. a kind of preparation method of nickel burst size examination criteria product according to claim 1, it is characterized in that: the mass ratio of described brass powder and nickel powder is 100:5 and 100:2.5.
3. a kind of preparation method of nickel burst size examination criteria product according to claim 1, it is characterized in that: the purity of brass powder is: 80～95%.
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| CN201310343581.4A CN103471880B (en) | 2013-08-08 | 2013-08-08 | Nickel release detection standard substance preparation method |
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| CN201310343581.4A CN103471880B (en) | 2013-08-08 | 2013-08-08 | Nickel release detection standard substance preparation method |
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| CN103471880A true CN103471880A (en) | 2013-12-25 |
| CN103471880B CN103471880B (en) | 2015-05-27 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105424903A (en) * | 2015-12-29 | 2016-03-23 | 许菲菲 | Method for rapidly detecting nickel release amount in alloy product |
| CN105758682A (en) * | 2016-02-01 | 2016-07-13 | 许菲菲 | Preparation method of standard substance for detecting harmful heavy metal in ornaments |
| CN107916341A (en) * | 2017-11-29 | 2018-04-17 | 江苏鑫海铜业有限公司 | A kind of alloyed copper bar preparation method |
| CN114459850A (en) * | 2021-12-23 | 2022-05-10 | 广州海关技术中心 | Preparation method of standard sample for detecting nickel release amount of ornament |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201732023U (en) * | 2010-08-11 | 2011-02-02 | 成都市产品质量监督检验院 | Metal fastener nickel release detecting preprocessing tester |
-
2013
- 2013-08-08 CN CN201310343581.4A patent/CN103471880B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201732023U (en) * | 2010-08-11 | 2011-02-02 | 成都市产品质量监督检验院 | Metal fastener nickel release detecting preprocessing tester |
Non-Patent Citations (1)
| Title |
|---|
| 英国标准学会: "《BS EN 1811-1998 Reference test method for release of nickel from products intended to come into direct and prolonged contact with the skin》", 15 April 1999 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105424903A (en) * | 2015-12-29 | 2016-03-23 | 许菲菲 | Method for rapidly detecting nickel release amount in alloy product |
| CN105424903B (en) * | 2015-12-29 | 2018-03-30 | 许菲菲 | Method for rapidly detecting nickel release amount in alloy product |
| CN105758682A (en) * | 2016-02-01 | 2016-07-13 | 许菲菲 | Preparation method of standard substance for detecting harmful heavy metal in ornaments |
| CN107916341A (en) * | 2017-11-29 | 2018-04-17 | 江苏鑫海铜业有限公司 | A kind of alloyed copper bar preparation method |
| CN114459850A (en) * | 2021-12-23 | 2022-05-10 | 广州海关技术中心 | Preparation method of standard sample for detecting nickel release amount of ornament |
| CN114459850B (en) * | 2021-12-23 | 2023-10-03 | 广州海关技术中心 | Preparation method of standard sample for detecting nickel release amount of ornaments |
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| CN103471880B (en) | 2015-05-27 |
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