CN103471880B - Nickel release detection standard substance preparation method - Google Patents
Nickel release detection standard substance preparation method Download PDFInfo
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- CN103471880B CN103471880B CN201310343581.4A CN201310343581A CN103471880B CN 103471880 B CN103471880 B CN 103471880B CN 201310343581 A CN201310343581 A CN 201310343581A CN 103471880 B CN103471880 B CN 103471880B
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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 and manufactures jewellery, coin, Metal buttons etc., and nickel is the modal reason causing contact allergy, about has the women of 10% ~ 20% can produce allergy to nickel.Skin Long-term absorption from directly with the nickel ion that discharges the nickel-containing material of skin contact, produce allergy, be exposed to further in soluble nickel salt and can produce Allergic contact dermatitis.European Parliament and EU Council instruction 94/27/EC(OJ No.L188 of 22.7.94) the rate of release threshold value of regulation nickel is 0.5 μ g/cm
2week.
Domestic at present have many third party testing agencies in the test carrying out nickel burst size, but it is domestic at present still without the standard items that nickel burst size detects, the standard items that nickel burst size conventional at present detects are generally from external import, obtain with gold and nickel mixing, cost is higher, and its homogeneity and stability await further raising.
Summary of the invention
The object of this invention is to provide a kind of preparation method of nickel burst size examination criteria product, the method technique is simple, produces workable, simple operation; Low with the standard items cost that this method is produced, material is easy to get, more easily the 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: by brass powder and nickel powder Homogeneous phase mixing in certain proportion, be mixed with presmelting raw material;
(2) melting: a) about the 1kg presmelting raw material of step (1) gained is placed in graphite crucible, adds layer of active carbon powder in case oxidation on presmelting raw material surface, then be positioned in Medium frequency induction equipment; B) setting initial induction current is 70 ± 5 A, adds hot smelting, in fusion process, stirs with graphite rod, stirs once every 2 minutes, continues about 3 ~ 5 minutes; C) turning down current value to 50 ± 5 A when evaporating more violent, continuing about 1 ~ 2 minute; D) step b, c carry out operation 3 times repeatedly, carry out argon shield in process; E) pour into a mould before melt and heighten current value to 80 A, heat 0.5 ~ 1 minute, and stir with graphite rod, then rapid by melt cast in graphite jig, make it cooling and make pole shape;
(3) cutting polishing: sheet specimens a) mode of the round bar samples spark cutting smelted and poured into a mould being cut into Φ 20 × 1.3 mm; B) polishing specimen surface to thickness with No. 400 adamas sand paper is 1.2mm, and sheet is 3.0g heavily about; The sample alcohol washes of c) will polish, hot blast drying, obtains 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, with the obtained A sample standard items of 5% and the B sample standard items of 2%.
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, produces workable, simple operation; Low with the standard items cost that this method is produced, material is easy to get, more easily the marketization, and homogeneity and good stability.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
The preparation of the A sample standard items of 5%.
(1) preparation of raw material: by brass powder with nickel powder with the quality of 100:5 than Homogeneous phase mixing, be mixed with presmelting raw material;
(2) melting: a) about the 1kg presmelting raw material of step (1) gained is placed in graphite crucible, adds layer of active carbon powder in case oxidation on presmelting raw material surface, then be positioned in Medium frequency induction equipment; B) setting initial induction current is 75 A, adds hot smelting, in fusion process, stirs with graphite rod, stirs once every 2 minutes, continues about 3 minutes; C) turning down current value to 50 A when evaporating more violent, continuing about 2 minutes; D) step b, c carry out operation 3 times repeatedly, carry out argon shield in process; E) pour into a mould before melt and heighten current value to 80 A, heat 1 minute, and stir with graphite rod, then rapid by melt cast in graphite jig, make it cooling and make pole shape;
(3) cutting polishing: sheet specimens a) mode of the round bar samples spark cutting smelted and poured into a mould being cut into Φ 20 × 1.3 mm; B) polishing specimen surface to thickness with No. 400 adamas sand paper is 1.2mm, and sheet is 3.0g heavily about; The sample alcohol washes of c) will polish, hot blast drying, obtains the A sample standard items of 5%.
Embodiment 2
The preparation of the B sample standard items of 2%.
(1) preparation of raw material: by brass powder with nickel powder with the quality of 100:2.5 than Homogeneous phase mixing, be mixed with presmelting raw material;
(2) melting: a) about the 1kg presmelting raw material of step (1) gained is placed in graphite crucible, adds layer of active carbon powder in case oxidation on presmelting raw material surface, then be positioned in Medium frequency induction equipment; B) setting initial induction current is 70 A, adds hot smelting, in fusion process, stirs with graphite rod, stirs once every 2 minutes, continues about 5 minutes; C) turning down current value to 52 A when evaporating more violent, continuing about 2 minutes; D) step b, c carry out operation 3 times repeatedly, carry out argon shield in process; E) pour into a mould before melt and heighten current value to 80 A, heat 0.5 minute, and stir with graphite rod, then rapid by melt cast in graphite jig, make it cooling and make pole shape;
(3) cutting polishing: sheet specimens a) mode of the round bar samples spark cutting smelted and poured into a mould being cut into Φ 20 × 1.3 mm; B) polishing specimen surface to thickness with No. 400 adamas sand paper is 1.2mm, and sheet is 3.0g heavily about; The sample alcohol washes of c) will polish, hot blast drying, obtains the B sample standard items of 2%.
In order to prove superiority of the present invention further, carried out the detection of homogeneity and stability to the standard items that the present invention produces, homogeneity and stability are the important parameters judging nickel burst size examination criteria product quality, decide 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 often group sample extracted, measure 2 times with random order under the same conditions, adopt one-factor analysis of variance method to carry out statistical treatment to the result after inspection.Assay (result of calculation presses EN1811:2011, does not carry out coefficient correction to testing result) is as shown in (table one).
Table one standard items uniformity data summary sheet
As shown in Table 1, wherein the F value of A sample standard items is the F value of 1.15, B sample standard items is 1.56, passes through
fdistribution table checks in
f 0.05the F value of (9,10)=3.02, A sample standard items and B sample standard items is all less than
f 0.05(9,10), show in the fiducial interval of 95%, the nickel burst size there was no significant difference of sample room, having good uniformity of sample.
In order to prove having good uniformity of the standard items that the present invention produces further, following spy provides from the uniformity testing data of the nickel burst size examination criteria product of foreign procurement that (result of calculation is by EN1811:2011, coefficient correction is not carried out to testing result), as shown in (table two).
The standard items uniformity data summary sheet of table two foreign procurement
As can be seen from Table II, the standard items of foreign procurement have extracted 10 groups of samples equally and have tested, the F value of its uniformity testing is 2.61, and the F value of the A sample standard items prepared 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, F value is larger, and sample is more uneven, this shows that the homogeneity of the standard items prepared with the present invention is better than the standard items of foreign procurement.
Two, the stability test of standard items
The A sample standard items of random selecting 6 part 5% are used for the inspection of stability, adopt
tmethod of inspection, comparative experiments room measures the consistance between two mean values obtaining.Stability has been carried out 5 times and has been detected, and time total span is 145 days, covers whole sense cycle 5 testing results, and each test result and on June 8th, 2012 are detected Comparative result 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, is all less than t
0.05(10)=2.228, show when 0.05 level of signifiance, and A sample standard items are stable in sense cycle.
As can be seen from above check data, the standard items homogeneity utilizing the present invention to produce and having good stability, fully can meet the detection demand of nickel burst size, and cost is low, and production technology is simple, easily prepares, can be promoted widely and apply.
Claims (3)
1. a preparation method for nickel burst size examination criteria product, comprises following three steps:
(1) preparation of raw material: by brass powder and nickel powder Homogeneous phase mixing in certain proportion, be mixed with presmelting raw material;
(2) melting: a) about the 1kg presmelting raw material of step (1) gained is placed in graphite crucible, adds layer of active carbon powder in case oxidation on presmelting raw material surface, then be positioned in Medium frequency induction equipment; B) setting initial induction current is 70 ± 5 A, adds hot smelting, in fusion process, stirs with graphite rod, stirs once every 2 minutes, continues 3 ~ 5 minutes; C) turn down current value to 50 ± 5 A when evaporating more violent, continue 1 ~ 2 minute, d) step b, c carry out operation 3 times repeatedly, carry out argon shield in process; E) pour into a mould before melt and heighten current value to 80 A, heat 0.5 ~ 1 minute, and stir with graphite rod, then rapid by melt cast in graphite jig, make it cooling and make pole shape;
(3) cutting polishing: sheet specimens a) mode of the round bar samples spark cutting smelted and poured into a mould being cut into Φ 20 × 1.3 mm; B) polishing specimen surface to thickness with No. 400 adamas sand paper is 1.2mm, and sheet is 3.0g heavily about; The sample alcohol washes of c) will polish, hot blast drying, obtains nickel burst size examination criteria product.
2. the preparation method of a kind of nickel burst size examination criteria product according to claim 1, is characterized in that: the mass ratio of described brass powder and nickel powder is 100:5 or 100:2.5.
3. the preparation method of a kind of nickel burst size examination criteria product according to claim 1, 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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| 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 |
| 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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