CN113295573B - Method for detecting gold content of electroformed hard gold product - Google Patents
Method for detecting gold content of electroformed hard gold product Download PDFInfo
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- CN113295573B CN113295573B CN202110559791.1A CN202110559791A CN113295573B CN 113295573 B CN113295573 B CN 113295573B CN 202110559791 A CN202110559791 A CN 202110559791A CN 113295573 B CN113295573 B CN 113295573B
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- 239000010931 gold Substances 0.000 title claims abstract description 98
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 97
- 238000000034 method Methods 0.000 title claims abstract description 30
- 230000004580 weight loss Effects 0.000 claims abstract description 51
- 238000005303 weighing Methods 0.000 claims abstract description 19
- 238000010998 test method Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims description 13
- 238000005520 cutting process Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000012952 Resampling Methods 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 26
- 238000012360 testing method Methods 0.000 abstract description 11
- 229910052751 metal Inorganic materials 0.000 abstract description 6
- 230000007547 defect Effects 0.000 abstract description 4
- 238000001506 fluorescence spectroscopy Methods 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 abstract description 3
- 238000012544 monitoring process Methods 0.000 abstract description 3
- 238000007747 plating Methods 0.000 abstract description 3
- 238000011410 subtraction method Methods 0.000 abstract description 3
- 239000000919 ceramic Substances 0.000 description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 4
- 238000011109 contamination Methods 0.000 description 3
- 239000004519 grease Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000011895 specific detection Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 229910052785 arsenic Inorganic materials 0.000 description 2
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 238000004846 x-ray emission Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005323 electroforming Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910000464 lead oxide Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention relates to a method for detecting gold content of an electroformed hard gold product, which comprises the following steps: selecting a crucible and carrying out constant weight on the crucible; weighing and calculating the weightlessness coefficient of the sample; and judging the gold content condition of the sample according to the weight loss coefficient. The method is simple to operate, short in period, capable of detecting a large number of samples simultaneously, relatively good in result accuracy, and convenient and quick in new method for controlling the gold content of the product for quality monitoring departments of factories. Compared with a fluorescence spectrometry and an ICP subtraction method, the method solves the defect that organic matters and light elements cannot be detected in principle; the vacuum furnace is skillfully adopted to remove volatile metal, organic matters and light elements in the electroformed hard gold ornament plating layer, compared with a fire test method, the operation flow is simplified, the detection time period is shortened (the detection time period is shortened from 6-8 hours to about 1 hour), the result is relatively accurate, and an uncertain sample can be subjected to fire test rechecking. Greatly reduces the cost, labor and workload of fire test experiments.
Description
Technical Field
The invention relates to hard gold purity detection, in particular to a detection method for gold content of an electroformed hard gold product.
Background
The electroformed (Three Dimension) hard gold jewelry is a new variety appearing in the jewelry market in recent years, the gold content is required to be more than or equal to 99.9 percent (namely Au per mill is more than or equal to 999 per mill), the electroformed hard gold jewelry is mainly produced by adopting an electroforming process, the electroformed hard gold jewelry has a plurality of excellent characteristics, the hardness and the wear resistance of gold are greatly improved, the hardness of electroformed hard gold is 2 to 3 times that of common gold, and the problem of softness and easy deformation of the texture of gold is solved. The gold ornament market is rapidly preempted once the gold ornament is pushed out. However, with the advent of hard gold products in large numbers, various inspection mechanisms have encountered a number of problems in the actual inspection process.
Currently, three main detection methods are an inductively coupled plasma atomic emission spectrometry (ICP-AES method), an X-ray fluorescence spectrometry and a fire test method. The combined product production process sample possibly contains elements such as carbon, nitrogen, arsenic, sulfur, phosphorus, light metal elements potassium, sodium and the like, but the detection of the elements such as carbon, nitrogen, arsenic, sulfur, phosphorus, light metal elements potassium, sodium and the like is not carried out in the current ICP-AES national standards (GB/T21198.6-2007, GB/T21198.4-2007 and GB/T11066.8), so that the result of detecting the content of relevant metal impurity elements in hard gold by adopting an ICP-AES method and obtaining the gold content by 100% difference is high. In the case of measurement by the X-ray fluorescence spectrometry, the non-metal and light elements cannot be measured due to limitations of the apparatus, the method itself and the standard sample, and therefore the detected gold content is also high (because the gold content is indirectly obtained by the normalization method). The conventional fire test method has long detection time, and generally requires 6-8 hours; the detection process uses a large amount of lead oxide, so that the operation environment is poor and the damage to the body is particularly large. Standard gold is used in the detection process, and the detection cost is high.
However, hard gold product customers have very strict requirements on the delivery period, and how to scientifically, rapidly and accurately detect the gold content of the product has become one of the most important links in production.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for detecting the gold content of an electroformed hard gold product.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a method for detecting gold content of an electroformed hard gold product, the method comprising:
selecting a crucible and carrying out constant weight on the crucible;
weighing and calculating the weightlessness coefficient of the sample;
and judging the gold content condition of the sample according to the weight loss coefficient.
The further technical scheme is as follows: the step of selecting a crucible and carrying out constant weight on the crucible specifically comprises the following steps:
selecting two crucibles with the same specification, and numbering the two crucibles as a first crucible and a second crucible;
placing the first crucible and the second crucible in a vacuum furnace with controllable temperature for multiple constant temperature, and determining whether the constant weight is finished according to the last two constant temperature conditions;
after the constant weight is completed, the first crucible and the second crucible are placed in a drying container to be preserved for standby.
The further technical scheme is as follows: the method comprises the steps of placing the first crucible and the second crucible in a temperature-controllable vacuum furnace for multiple constant temperature, and determining whether the constant weight is finished according to the last two constant temperature conditions, wherein the method specifically comprises the following steps:
placing the first crucible and the second crucible in a vacuum furnace, and keeping the temperature at 500 ℃ for 2 hours;
placing the first crucible and the second crucible in a vacuum furnace again, and keeping the temperature at 800 ℃ for 2 hours;
placing the first crucible and the second crucible in a vacuum furnace again, keeping the temperature at 1000 ℃ for 2 hours, and repeating at least twice under the condition of keeping the temperature at 1000 ℃ for 2 hours;
measuring whether the difference between the weights of the first crucible and the second crucible at a constant temperature of 1000 ℃ for 2 hours is within a specified range;
if the weight of the first crucible and the second crucible is within the specified range, the constant weight of the first crucible and the second crucible is completed.
The further technical scheme is as follows: in the step of measuring whether or not the difference between the weights of the first crucible and the second crucible at a constant temperature of 1000 ℃ for 2 hours is within a prescribed range, the prescribed range is 0.2mg or less.
The further technical scheme is as follows: the step of weighing and calculating the weight loss coefficient of the sample specifically comprises the following steps:
cutting the electroformed hard gold ornaments into small slices, and uniformly mixing;
two parallel samples are weighed from the electroformed hard gold ornament cut into small pieces and numbered as a first sample and a second sample, and the weight m of the first sample is recorded A And weight m of the second sample B 。
Placing a first sample in a first crucible with constant weight, placing a second sample in a second crucible with constant weight, and recording the total weight m of the first crucible with the first sample 1 And the total weight m of the second crucible containing the second sample 2 ；
Placing a first crucible containing a first sample and a second crucible containing a second sample in a vacuum furnace, and keeping the temperature at 1000 ℃ for 30 minutes;
taking out the first crucible containing the first sample and the second crucible containing the second sample from the vacuum furnace, placing the first crucible and the second crucible in a drying container, naturally cooling the crucible and recording the total weight m of the first crucible containing the first sample 3 And the total weight m of the second crucible containing the second sample 4 。
According to m A 、m B 、m 1 、m 2 、m 3 And m 4 Calculating the weight loss coefficient of the sample
The further technical scheme is as follows: said according to m A 、m B 、m 1 、m 2 、m 3 And m 4 Calculating the weight loss coefficient of the sampleIn the step (a), the adopted calculation formula is as follows:
wherein (1)>For the weight loss coefficient of the first sample, +.>For the weight loss coefficient of the second sample, +.>Is the average weight loss coefficient of two samples.
The further technical scheme is as follows: the step of judging the gold content condition of the sample according to the weightlessness coefficient specifically comprises the following steps:
judging the average weightlessness coefficientWhether or not to be equal to or greater than 999.5;
if the weight loss coefficient is averaged999.5, judging that the gold content of the electroformed hard gold ornament is larger than Au999;
if not, judging the average weightlessness coefficientWhether or not to useLess than 999.0;
if the weight loss coefficient is averagedAnd if the gold content is smaller than 999.0, judging that the gold content of the electroformed hard gold ornament is smaller than Au999.
The further technical scheme is as follows: the step of determining the gold content of the sample according to the weight loss coefficient further comprises the following steps:
if the weight loss coefficient is averagedLess than 999.5 and greater than 999.0, resampling, and determining the gold content of the electroformed hard gold ornament by adopting a fire gold test method.
Compared with the prior art, the invention has the beneficial effects that: the invention can rapidly measure the result in a weighing and calculating mode, has simple operation and short period, can detect a large number of samples at the same time, has relatively good result accuracy, and provides a novel method for controlling the gold content of the product for a factory quality monitoring department. Compared with a fluorescence spectrometry and an ICP subtraction method, the method solves the defect that organic matters and light elements cannot be detected in principle; the vacuum furnace is skillfully adopted to remove volatile metal, organic matters and light elements in the electroformed hard gold ornament plating layer, compared with a fire test method, the operation flow is simplified, the detection time period is shortened (the detection time period is shortened from 6-8 hours to about 1 hour), the result is relatively accurate, and an uncertain sample can be subjected to fire test rechecking. Greatly reduces the cost, labor and workload of fire test experiments.
The foregoing description is only an overview of the present invention, and is intended to be more clearly understood as being carried out in accordance with the following description of the preferred embodiments, as well as other objects, features and advantages of the present invention.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph showing the comparison of the results of the detection of gold content of samples obtained by different detection methods by sampling and detecting the same sample according to GB/T18043-2013, GB/T9288-2019 and the method.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below in conjunction with specific embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be understood that the terms "comprises" and "comprising," when used in this specification and the appended claims, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
It is also to be understood that the terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in this specification and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
It should be further understood that the term "and/or" as used in the present specification and the appended claims refers to any and all possible combinations of one or more of the associated listed items, and includes such combinations.
The invention discloses a method for detecting gold content of electroformed hard gold products, which comprises the following steps of: the crucible is a ceramic crucible, and a platinum crucible, a porcelain crucible, a stainless steel crucible and the like can be selected in actual test. The vacuum furnace is a temperature-controllable vacuum furnace, and a container such as a resistance furnace which can be heated to 1000 ℃ can be selected in actual test. The drying container is a glass vessel.
Example 1
In this embodiment, a heart-shaped pendant of an electroformed hard gold ornament is selected as a detection sample, and the specific detection steps are as follows:
s10, selecting 250mL two ceramic crucibles (a first crucible and a second crucible respectively), and keeping the weight constant; the specific steps of S10 are as follows:
s101, placing a ceramic crucible in a vacuum furnace by using a clean crucible clamp (the crucible clamp is used for avoiding direct contact by hands and avoiding grease contamination of the crucible), and keeping the temperature at 500 ℃ for 2 hours (the first constant weight must be sufficiently aged, and the heating speed cannot be too high);
s102, placing the two crucibles in a vacuum furnace, and keeping the temperature at 800 ℃ for 2 hours;
s103, placing the two crucibles in a vacuum furnace, keeping the temperature at 1000 ℃ for 2 hours, taking out, and then placing the crucibles in a dry glassware for natural cooling; the ceramic crucible was weighed using a one-ten-thousandth balance, where the first crucible weight was 11191.12mg and the second crucible weight was 11108.65mg;
s104, placing the two crucibles in a vacuum furnace, keeping the temperature at 1000 ℃ for 2 hours, taking out, and then placing the crucibles in a dry glassware for natural cooling; the ceramic crucible was weighed using a one-ten-thousandth balance, where the first crucible weight was 11191.12mg and the second crucible weight was 11108.65mg;
s105, after the temperature is kept at 1000 ℃ for 2 hours for 2 times, the weight difference obtained by weighing the first crucible and the second crucible twice is 0 (not exceeding the specified range, namely 0.02 mg), so that the constant weight of the two crucibles is finished, and the two crucibles are put into a dry glassware for storage for standby.
S20, weighing and calculating the weight loss coefficient of the sample; the specific steps of S20 are as follows:
s201, cutting the electroformed hard gold ornament heart-shaped pendant into small slices (1 mm), and uniformly mixing;
s202, slaveTwo samples (first and second samples) were weighed from the chopped flakes, and the weights were: first sample m A :200.10mg, second sample m B ：200.30mg；
S203, placing the first sample in a first crucible, placing the second sample in a second crucible, wherein the total weight m of the first sample and the first crucible 1 11391.22mg, total weight of second sample and second crucible m 2 11308.95mg;
s204, placing the first crucible and the second crucible in a vacuum furnace at 1000 ℃ and keeping the temperature constant for 30min;
s205, taking out the two crucibles, placing the two crucibles in a dry glassware, naturally cooling the two crucibles, and weighing the two crucibles, wherein the total weight m of the first sample and the first crucible is equal to the total weight m 3 11391.14mg, the total weight m4 of the second sample and the second crucible being 11308.89mg;
s206, according to m A 、m B 、m 1 、m 2 、m 3 And m 4 Calculating the weight loss coefficient of the sample
The calculation formula adopted by the calculation is as follows:
wherein (1)>For the weight loss coefficient of the first sample, +.>Is the second oneWeight loss coefficient of sample, +.>Is the average weight loss coefficient of two samples.
The result of the calculation is:
weight loss coefficient of first sample
Weight loss coefficient of the second sample
Average weight loss coefficient of two samples
S30, judging the gold content condition of the sample according to the weightlessness coefficient;
because the average weight loss coefficient of the two samples is 999.65 per mill, the gold content of the electroformed hard gold jewelry heart-shaped pendant in the embodiment is more than 999.0 per mill (namely, the gold content is more than or equal to 999 per mill), and the gold content meets the requirement of electroformed hard gold jewelry.
Example two
In the embodiment, an electroformed hard gold ornament Pixiu is selected as a detection sample, and the specific detection steps are as follows:
s10, selecting 250mL two ceramic crucibles (a first crucible and a second crucible respectively), and keeping the weight constant; the specific steps of S10 are as follows:
s101, placing a ceramic crucible in a vacuum furnace by using a clean crucible clamp (the crucible clamp is used for avoiding direct contact by hands and avoiding grease contamination of the crucible), and keeping the temperature at 500 ℃ for 2 hours (the first constant weight must be sufficiently aged, and the heating speed cannot be too high);
s102, placing the two crucibles in a vacuum furnace, and keeping the temperature at 800 ℃ for 2 hours;
s103, placing the two crucibles in a vacuum furnace, keeping the temperature at 1000 ℃ for 2 hours, taking out, and then placing the crucibles in a dry glassware for natural cooling; the ceramic crucible was weighed using a one-ten-thousandth balance, where the first crucible weight was 11191.12mg and the second crucible weight was 11108.65mg;
s104, placing the two crucibles in a vacuum furnace, keeping the temperature at 1000 ℃ for 2 hours, taking out, and then placing the crucibles in a dry glassware for natural cooling; the ceramic crucible was weighed using a one-ten-thousandth balance, where the first crucible weight was 11190.82mg and the second crucible weight was 11108.24mg;
s1041, placing the two crucibles in a vacuum furnace, keeping the temperature at 1000 ℃ for 2 hours, taking out, and then placing the crucibles in a dry glassware for natural cooling; the ceramic crucible was weighed using a one-ten-thousandth balance, where the first crucible weight was 11190.82mg and the second crucible weight was 11108.24mg;
s105, after the temperature is kept at 1000 ℃ for 2 hours for 3 times, the weight difference obtained by weighing the first crucible and the second crucible twice is 0 (not exceeding the specified range, namely 0.02 mg), so that the constant weight of the two crucibles is finished, and the two crucibles are put into a dry glassware for storage for standby.
S20, weighing and calculating the weight loss coefficient of the sample; the specific steps of S20 are as follows:
s201, cutting the electroformed hard gold ornament Pixiu (1 mm) into small slices, and uniformly mixing;
s202, weighing two samples (a first sample and a second sample) from the sheared small slices, wherein the weights of the two samples are respectively as follows: first sample m A :400.85mg, second sample m B ：400.76mg；
S203, placing the first sample in a first crucible, placing the second sample in a second crucible, wherein the total weight m of the first sample and the first crucible 1 11591.67mg, total weight of second sample and second crucible m 2 11509.00mg;
s204, placing the first crucible and the second crucible in a vacuum furnace at 1000 ℃ and keeping the temperature constant for 30min;
s205, taking out the two crucibles, placing the two crucibles in a dry glassware, naturally cooling the two crucibles, and weighing the two crucibles, wherein the total weight m of the first sample and the first crucible is equal to the total weight m 3 11591.24mg, the total weight m4 of the second sample and the second crucible being 11508.53mg;
s206, according to m A 、m B 、m 1 、m 2 、m 3 And m 4 Calculating the weight loss coefficient of the sample
The calculation formula adopted by the calculation is as follows:
wherein (1)>For the weight loss coefficient of the first sample, +.>For the weight loss coefficient of the second sample, +.>Is the average weight loss coefficient of two samples.
The result of the calculation is:
weight loss coefficient of first sample
Weight loss coefficient of the second sample
Average weight loss coefficient of two samples
S30, judging the gold content condition of the sample according to the weightlessness coefficient;
because the average weight loss coefficient of the two samples is 998.88 per mill, the gold content of the electroformed hard gold jewelry in the embodiment is 998.88 per mill (namely, the gold content is less than 999 per mill), and the gold content does not meet the requirement of the electroformed hard gold jewelry.
Example III
In this embodiment, the electroformed hard gold decorative bracelet is selected as a detection sample, and the specific detection steps are as follows:
s10, selecting 250mL two ceramic crucibles (a first crucible and a second crucible respectively), and keeping the weight constant; the specific steps of S10 are as follows:
s101, placing a ceramic crucible in a vacuum furnace by using a clean crucible clamp (the crucible clamp is used for avoiding direct contact by hands and avoiding grease contamination of the crucible), and keeping the temperature at 500 ℃ for 2 hours (the first constant weight must be sufficiently aged, and the heating speed cannot be too high);
s102, placing the two crucibles in a vacuum furnace, and keeping the temperature at 800 ℃ for 2 hours;
s103, placing the two crucibles in a vacuum furnace, keeping the temperature at 1000 ℃ for 2 hours, taking out, and then placing the crucibles in a dry glassware for natural cooling; the ceramic crucible was weighed using a one-ten-thousandth balance, where the first crucible weight was 12477.46mg and the second crucible weight was 10996.49mg;
s104, placing the two crucibles in a vacuum furnace, keeping the temperature at 1000 ℃ for 2 hours, taking out, and then placing the crucibles in a dry glassware for natural cooling; the ceramic crucible was weighed using a one-ten-thousandth balance, where the first crucible weight was 12477.08mg and the second crucible weight was 10995.86mg;
s1041, placing the two crucibles in a vacuum furnace, keeping the temperature at 1000 ℃ for 2 hours, taking out, and then placing the crucibles in a dry glassware for natural cooling; the ceramic crucible was weighed using a one-ten-thousandth balance, where the first crucible weight was 12477.08mg and the second crucible weight was 10995.86mg;
s105, after the temperature is kept at 1000 ℃ for 2 hours for 3 times, the weight difference obtained by weighing the first crucible and the second crucible twice is 0 (not exceeding the specified range, namely 0.02 mg), so that the constant weight of the two crucibles is finished, and the two crucibles are put into a dry glassware for storage for standby.
S20, weighing and calculating the weight loss coefficient of the sample; the specific steps of S20 are as follows:
s201, cutting the electroformed hard gold ornament bracelets into small sheets (1 mm is 1 mm), and uniformly mixing;
s202, weighing two samples (a first sample and a second sample) from the sheared small slices, wherein the weights of the two samples are respectively as follows: first sample m A :590.47mg, second sample m B ：590.45mg；
S203, placing the first sample in a first crucible, placing the second sample in a second crucible, wherein the total weight m of the first sample and the first crucible 1 13067.55mg, total weight of second sample and second crucible m 2 11586.31mg;
s204, placing the first crucible and the second crucible in a vacuum furnace at 1000 ℃ and keeping the temperature constant for 30min;
s205, taking out the two crucibles, placing the two crucibles in a dry glassware, naturally cooling the two crucibles, and weighing the two crucibles, wherein the total weight m of the first sample and the first crucible is equal to the total weight m 3 13066.66mg, the total weight m4 of the second sample and the second crucible being 11585.37mg;
s206, according to m A 、m B 、m 1 、m 2 、m 3 And m 4 Calculating the weight loss coefficient of the sample
The calculation formula adopted by the calculation is as follows:
wherein (1)>For the weight loss coefficient of the first sample, +.>For the weight loss coefficient of the second sample, +.>Is the average weight loss coefficient of two samples.
The result of the calculation is:
weight loss coefficient of first sample
Weight loss coefficient of the second sample
Average weight loss coefficient of two samples
S30, judging the gold content condition of the sample according to the weightlessness coefficient;
because the average weight loss coefficient of the two samples is 998.45 per mill, the gold content of the electroformed hard gold jewelry in the embodiment is 998.45 per mill (namely, the gold content is less than 999 per mill), and the gold content does not meet the requirement of the electroformed hard gold jewelry.
In order to better illustrate that the detection method of the present invention is superior to the existing detection method, please refer to fig. 1, fig. 1 is a comparison chart of detection results of gold content of samples obtained by comparing different detection methods according to the methods of GB/T18043-2013 and GB/T9288-2019, and the same sample is sampled and detected respectively.
As can be seen from Table 2 and FIG. 1, the difference between the results is large when different detection methods are selected for the same electroformed hard gold ornament. The overall law is: for the gold content of the same sample, the fluorescence spectrometry of the detection result is larger than the quick detection method and larger than the fire test method (arbitration method). The comparison of the method and the fire test method can show that: when the weight loss coefficient is more than or equal to 999.5, the fire test result of the product is more than or equal to 999.0; resampling when 999.0 is less than or equal to the weight loss coefficient less than 999.5, and taking the fire test result as the reference; when the weight loss coefficient is less than 999.0, the fire test result of the product is less than 999.0.
To sum up: the invention can rapidly measure the result in a weighing and calculating mode, has simple operation and short period, can detect a large number of samples at the same time, has relatively good result accuracy, and provides a novel method for controlling the gold content of the product for a factory quality monitoring department. Compared with a fluorescence spectrometry and an ICP subtraction method, the method solves the defect that organic matters and light elements cannot be detected in principle; the vacuum furnace is skillfully adopted to remove volatile metal, organic matters and light elements in the electroformed hard gold ornament plating layer, compared with a fire test method, the operation flow is simplified, the detection time period is shortened (the detection time period is shortened from 6-8 hours to about 1 hour), the result is relatively accurate, and an uncertain sample can be subjected to fire test rechecking. Greatly reduces the cost, labor and workload of fire test experiments.
While the invention has been described with reference to certain preferred embodiments, it will be understood by those skilled in the art that various changes and substitutions of equivalents may be made and equivalents will be apparent to those skilled in the art without departing from the scope of the invention. Therefore, the protection scope of the invention is subject to the protection scope of the claims.
Claims (1)
1. The method for detecting the gold content of the electroformed hard gold product is characterized by comprising the following steps of:
selecting a crucible and carrying out constant weight on the crucible;
weighing and calculating the weightlessness coefficient of the sample;
judging the gold content condition of the sample according to the weight loss coefficient;
the step of selecting a crucible and carrying out constant weight on the crucible specifically comprises the following steps:
selecting two crucibles with the same specification, and numbering the two crucibles as a first crucible and a second crucible;
placing the first crucible and the second crucible in a vacuum furnace with controllable temperature for multiple constant temperature, and determining whether the constant weight is finished according to the last two constant temperature conditions;
after the constant weight is finished, the first crucible and the second crucible are placed in a drying container for standby;
the step of weighing and calculating the weight loss coefficient of the sample specifically comprises the following steps:
cutting the electroformed hard gold ornaments into small slices, and uniformly mixing;
weighing two parallel samples from the electroformed hard gold ornament cut into small pieces, numbering the samples as a first sample and a second sample, and recording the weight of the first sampleAnd the weight of the second sample->；
Placing the first sample in a first crucible with constant weight, placing the second sample in a second crucible with constant weight, and recording total weight of the first crucible with the first sampleAnd the total weight of the second crucible containing the second sample +.>；
Placing a first crucible containing a first sample and a second crucible containing a second sample in a vacuum furnace, and keeping the temperature at 1000 ℃ for 30 minutes;
taking out the first crucible containing the first sample and the second crucible containing the second sample from the vacuum furnace, placing the crucible in a drying container for natural cooling, and recording the total weight of the first crucible containing the first sampleAnd the total weight of the second crucible containing the second sample +.>；
According toAnd->Calculating the weight loss coefficient of the sample->；
Said basis isAnd->Calculating the weight loss coefficient of the sample->In the step (a), the adopted calculation formula is as follows:
;
;
wherein, the->For the weight loss coefficient of the first sample, +.>For the second sampleWeight loss coefficient of>The average weight loss coefficient of two samples;
the step of judging the gold content condition of the sample according to the weightlessness coefficient specifically comprises the following steps:
judging the average weightlessness coefficientWhether or not to be equal to or greater than 999.5;
if the weight loss coefficient is averaged999.5, judging that the gold content of the electroformed hard gold ornament is larger than Au999;
if not, judging the average weightlessness coefficientWhether or not less than 999.0;
if the weight loss coefficient is averagedIf the gold content of the electroformed hard gold ornament is less than 999.0, judging that the gold content of the electroformed hard gold ornament is less than Au999;
the method comprises the steps of placing the first crucible and the second crucible in a temperature-controllable vacuum furnace for multiple constant temperature, and determining whether the constant weight is finished according to the last two constant temperature conditions, wherein the method specifically comprises the following steps:
placing the first crucible and the second crucible in a vacuum furnace, and keeping the temperature at 500 ℃ for 2 hours;
placing the first crucible and the second crucible in a vacuum furnace again, and keeping the temperature at 800 ℃ for 2 hours;
placing the first crucible and the second crucible in a vacuum furnace again, keeping the temperature at 1000 ℃ for 2 hours, and repeating at least twice under the condition of keeping the temperature at 1000 ℃ for 2 hours;
measuring whether the difference between the weights of the first crucible and the second crucible at a constant temperature of 1000 ℃ for 2 hours is within a specified range;
if the weight of the first crucible and the weight of the second crucible are within the specified range, finishing the constant weight of the first crucible and the constant weight of the second crucible;
in the step of measuring whether the difference between the weights of the first crucible and the second crucible is within a prescribed range or not under the condition of keeping the temperature of 1000 ℃ for 2 hours, the prescribed range is 0.2mg or less;
the step of determining the gold content of the sample according to the weight loss coefficient further comprises the following steps:
if the weight loss coefficient is averagedLess than 999.5 and greater than 999.0, resampling, and determining the gold content of the electroformed hard gold ornament by adopting a fire gold test method.
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