CN111650081A - Method for measuring gold quality and harmful elements in gold of pure silver gold-plated jewelry - Google Patents
Method for measuring gold quality and harmful elements in gold of pure silver gold-plated jewelry Download PDFInfo
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Abstract
The invention belongs to the technical field of precious metal jewelry measurement, and particularly relates to a method for measuring gold quality and harmful elements in gold of a pure silver gold-plated jewelry; heating N, N-dimethylacetamide to remove the coating layer on the surface of the jewelry, uniformly cutting the jewelry into sections, dissolving silver in dilute nitric acid solution, separating gold, stabilizing and complexing the silver in ammonium chloride solution, removing impurities on the surface of the gold by acetone ultrasonic method, weighing the mass of the gold, dissolving the gold by aqua regia, and measuring harmful elements in the gold by ICP-AES method. The invention adopts N, N-dimethyl acetamide heating method to remove the coating layer on the jewelry surface, cuts the jewelry into uniform section shape, avoids the dispersion of gold in the silver removing process and is not easy to collect, the acetone ultrasonic method solves the adhesion of impurity elements on the gold surface, and the ammonium chloride solution is adopted to stably complex silver ions, thereby eliminating the influence of silver on the gold quality and the determination of harmful elements in gold.
Description
Technical Field
The invention belongs to the technical field of precious metal jewelry measurement, and particularly relates to a method for measuring gold quality and harmful elements in gold of pure silver gold-plated jewelry.
Background
Gold is an important precious metal, is always applied to currency, value-retaining objects and jewelry, is more widely applied to precious metal jewelry and is favored by consumers. The quality and purity of gold in jewelry affect the value-keeping price, so it is very important to accurately determine the quality and purity of gold in jewelry. Common jewelry comprises bracelets, rings, ear nails and the like, and in order to guarantee the legal rights and interests of consumers, the quality and purity of each precious metal jewelry need to be detected before sale, and relevant certificates are issued for sale. In order to reduce the production cost of the jewelry and keep the beautiful effect of the jewelry, jewelry manufacturers adopt a pure silver gold plating process to produce the jewelry, and the jewelry does not have a national standard detection method, thereby seriously influencing the development of a precious metal market.
The pure silver gold-plated jewelry is internally silver, the outer layer of the pure silver gold-plated jewelry is thin gold, and a part of coating layer is attached to the outer surface of some jewelry to achieve an attractive effect.
The quality of the precious metal jewelry is measured according to QB/T1690-2004 'Provisions on precious metal jewelry quality measurement tolerance', the standard is suitable for precious metal detection of a pure matrix and is not suitable for measuring the quality of gold in the pure silver gold-plated jewelry, because the pure silver gold-plated jewelry is formed by a layer of gold on the surface of pure silver, the quality of the pure gold cannot be measured independently. Nondestructive detection is carried out according to GB/T18043-2013X-ray fluorescence spectrometry for determining precious metal content of jewelry, the X-ray fluorescence spectrometry has the advantages of high analysis speed in precious metal jewelry analysis, no damage to a sample in the determination process, and poor measurement precision and accuracy, wherein the RSD is generally between 0.1% and 0.5%. In addition, in the analysis process, X-rays can penetrate through the surface of the metal to be tested, the thickness of the penetrating metal is generally not more than 10 microns, the tested pure gold sample is required to have better uniformity, and the phenomena of filling and wrapping are avoided, so that the X-ray fluorescence spectrometry is not suitable for being used as an arbitration analysis method for precious metal jewelry samples.
The safety of the noble metal jewelry as an ornament worn by people nearby is more and more concerned by people, so that the content of harmful elements in the noble metal jewelry is inspected, the market admission is strictly closed, the influence of the harmful elements on the human health is reduced or eliminated to the greatest extent, and the noble metal jewelry inspection method is the most important link in the inspection of the noble metal jewelry. The detection of harmful elements in noble metals is mandatory in many international fields, and the elements to be detected include arsenic, chromium, lead, mercury and cadmium, and besides, many harmful elements to be detected, such as nickel, bismuth, antimony, manganese, selenium, cobalt and the like. The inside of the pure silver gold-plated jewelry is silver, the outside is gold, and the gold is a part which is contacted with a human body, so that the harmful elements in the gold need to be accurately measured, and the physical and mental health of a wearer is protected.
In order to detect harmful elements, a sample needs to be rolled into a thin sheet (the thinner the sample is, the better the sample is), cut into pieces as much as possible and mixed uniformly, silver is removed by nitric acid for gold separation, so that gold is in dispersed pieces, gold cannot be completely collected, and the quality of the gold cannot be accurately measured; the silver matrix has high concentration, and the gold is very easy to attach to the inner surface of gold and is not easy to remove in the gold separation process, so that the quality of the gold cannot be accurately measured, and the measurement of harmful elements in the gold is influenced.
In conclusion, it is a difficult problem to accurately determine the quality of gold and the harmful elements in gold in the pure silver gold-plated jewelry.
Disclosure of Invention
In order to overcome the problems, the invention provides a method for measuring the quality of gold and harmful elements in gold in a pure silver gold-plated jewelry, which is particularly suitable for the pure silver gold-plated jewelry with the gold mass fraction of not less than 999 thousandths, aiming at the problem that the quality of gold and the harmful elements in gold in the pure silver gold-plated jewelry cannot be accurately measured at present, a method of cutting a sample into sections is adopted, silver is removed by dilute nitric acid, the problem that the gold is fragile in the silver dissolving process is solved, ammonium chloride is adopted to stabilize and complex the silver in the silver separating and removing process, the silver in the solution is thoroughly separated from the gold, and the inner surface and the outer surface of the pure gold are cleaned by an acetone ultrasonic method, so that the silver in the solution does not interfere with the measurement.
A method for measuring gold quality and harmful elements in gold of a pure silver gold-plated jewelry comprises the following steps:
putting the jewelry to be tested into a 400mL beaker, adding 50 mL-100 mL of N, N-dimethylacetamide reagent, heating on an electric stove plate until boiling, and keeping for 15 min-30 min;
pouring out the solution in the beaker treated in the step one, washing the jewelry to be detected for 3-5 times by using secondary deionized water, and heating and drying the jewelry to be detected;
thirdly, shearing the jewelry to be detected into uniform sections by using hydraulic pliers, wherein the length of each section is 1-1.5 cm, putting the jewelry to be detected into a 400mL beaker, adding 50-100 mL of dilute nitric acid solution, and heating the jewelry to be detected on an electric stove plate at the temperature of 200 ℃ until no small bubbles are generated;
taking out gold by using plastic tweezers, washing the gold taken out for 3-5 times by using a dilute nitric acid solution, washing the gold taken out for 3-5 times by using water, putting the gold taken out into a 250mL beaker, adding 30-50 mL of ammonium chloride solution, heating for 5-10 min, pouring out the solution in the beaker, washing the gold in the beaker for 3-5 times by using water, and then putting the washed gold back into the 250mL beaker;
step five, adding 30mL of acetone into the 250mL beaker obtained in the step four, and putting the beaker into an ultrasonic machine for ultrasonic treatment for 10 min;
and step six, pouring out the solution in the beaker after the ultrasonic treatment is finished, placing the beaker in an electric oven at 100 ℃ for heating for 30min, taking out the beaker, cooling to room temperature, placing the gold in the beaker on an analytical balance for weighing, and recording the mass of the gold as m1The gold quality in the jewelry to be detected is obtained;
step seven, the mass obtained in the step six is m1Weighing mass m in gold2Placing 0.2000g of sample gold in a 25mL volumetric flask, adding 5mL of aqua regia, heating until the sample gold is completely dissolved, cooling, adding water to a constant volume to scale, and uniformly mixing, wherein the solution in the volumetric flask is a sample to be detected, and the volume is marked as V;
step eight, carrying out a blank test along with the sample;
weighing four parts of 0.2000g of high-purity gold, respectively placing the four parts of high-purity gold in four 25mL volumetric flasks, respectively adding 5mL of aqua regia into the four 25mL volumetric flasks, respectively heating until the high-purity gold in the volumetric flasks is completely dissolved, respectively adding standard solutions containing nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury into the four 25mL volumetric flasks so that the concentrations of the standard solutions containing nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury in each volumetric flask are respectively 0.00ug/mL, 1.00ug/mL, 2.00ug/mL and 4.00ug/mL, respectively measuring the spectral line intensities of nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury in the four 25mL volumetric flasks by using an inductively coupled plasma emission spectrometer, respectively measuring the mass concentrations of eleven elements of nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury in the four 25mL volumetric flasks as horizontal coordinates, the spectral line intensity is a standard curve drawn by a vertical coordinate;
step ten: measuring the spectral line intensity of eleven elements of nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury in the 25mL volumetric flask in the seventh step by using an inductively coupled plasma emission spectrometer, and finding out the mass concentration of the eleven elements of nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury to be tested in the seventh step from the standard curve in the ninth step;
step eleven, calculating the content of the harmful elements to be detected in the gold in the jewelry to be detected according to the following formula:
in the formula: omegaiThe content of harmful elements to be detected, mk/kg, contained in the gold in the jewelry to be detected;
Cistep ten, finding out the sample to be tested from the standard curveMass concentration of harmful elements, ug/mL;
v is the volume of the sample to be measured, mL;
m2weighing the mass of sample gold in the gold contained in the jewelry to be detected, namely mg.
The preparation method of the dilute nitric acid solution used in the third step and the fourth step comprises the following steps: 50mL of nitric acid with ρ 1.42g/mL was weighed and added to 150mL of secondary deionized water, followed by mixing.
In the fourth step, the concentration of the ammonium chloride solution is 20 g/L.
The invention has the beneficial effects that:
1. the N, N-dimethylacetamide heating method is used for removing the coating layer on the surface of the jewelry, so that the problem of removing the jewelry coating layer is solved.
2. The jewelry sample is cut into uniform sections, the appearance shape of the sample is not damaged, and gold keeps the original shape in the process of separating pure silver from nitric acid, is easy to collect and is not broken.
3. The acetone ultrasonic method is adopted to solve the problem of attachment of substances such as impurity elements and organic matters on the surface of the gold, and the accuracy of the impurity elements in the gold is ensured.
4. The method can accurately and rapidly measure the impurity elements in the pure gold, adopts the ammonium chloride solution to stably complex silver ions, eliminates the influence of silver on the impurity measurement, and fills the blank of measuring the quality of gold and the harmful elements in the gold in the pure silver gold-plated jewelry.
Detailed Description
A method for measuring gold quality and harmful elements in gold of a pure silver gold-plated jewelry comprises the following steps:
putting the jewelry to be tested into a 400mL beaker, adding 50 mL-100 mL of N, N-dimethylacetamide reagent, heating on an electric stove plate until boiling, and keeping for 15 min-30 min;
pouring out the solution in the beaker treated in the step one, washing the jewelry to be detected for 3-5 times by using secondary deionized water, and heating and drying the jewelry to be detected;
thirdly, cutting the jewelry to be tested into uniform sections by using hydraulic pliers, wherein the length of each section is 1-1.5 cm, putting the jewelry to be tested into a 400mL beaker, adding 50-100 mL of dilute nitric acid solution, and heating the beaker on an electric stove plate at 200 ℃ until no small bubbles are generated, namely, all silver in the pure silver gold-plated jewelry to be tested is dissolved;
taking out gold by using plastic tweezers, washing the gold taken out for 3-5 times by using a dilute nitric acid solution, washing the gold taken out for 3-5 times by using water, then putting the gold taken out into a 250mL beaker, adding 30-50 mL of ammonium chloride solution into the 250mL beaker, heating for 5-10 min, pouring out the solution in the beaker, washing the gold in the beaker for 3-5 times by using water, and then putting the washed gold back into the 250mL beaker;
step five, adding 30mL of acetone into the 250mL beaker obtained in the step four, and putting the beaker into an ultrasonic machine for ultrasonic treatment for 10 min;
and step six, pouring out the solution in the beaker after the ultrasonic treatment is finished, placing the beaker in an electric oven at 100 ℃ for heating for 30min, taking out the beaker, cooling to room temperature, placing the gold in the beaker on an analytical balance for weighing, and recording the mass of the gold as m1The gold quality in the jewelry to be detected is obtained; (to the nearest 0.0001 g).
Step seven, the mass obtained in the step six is m1Weighing mass m in gold2Placing 0.2000g of sample gold in a 25mL volumetric flask, adding 5mL of aqua regia, heating until the sample gold is completely dissolved, cooling, adding water to a constant volume to scale, and uniformly mixing, wherein the solution in the volumetric flask is a sample to be detected, and the volume is marked as V;
step eight, carrying out a blank test along with the sample;
weighing four parts of 0.2000g of high-purity gold (gold with the purity of not less than 99.999%) and respectively placing the four parts of high-purity gold into four 25mL volumetric flasks, respectively adding 5mL of aqua regia into the four 25mL volumetric flasks, respectively heating until the high-purity gold in the volumetric flasks is completely dissolved, respectively adding standard solutions containing nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury into the four 25mL volumetric flasks so that the concentrations of the standard solutions containing nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury in each volumetric flask are respectively 0.00ug/mL, 1.00ug/mL, 2.00ug/mL and 4.00ug/mL, respectively measuring the spectral line intensities of nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury in the four 25mL volumetric flasks by using an inductively coupled plasma emission spectrometer, respectively measuring the spectral line intensities of nickel, bismuth, cadmium, cobalt, lead, antimony, chromium, arsenic, selenium and mercury, The mass concentration of eleven elements of arsenic, selenium and mercury is an abscissa, and the spectral line intensity is an ordinate to draw a standard curve;
step ten: measuring the spectral line intensity of eleven elements of nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury in the 25mL volumetric flask in the seventh step by using an inductively coupled plasma emission spectrometer, and finding out the mass concentration of the eleven elements of nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury to be tested in the seventh step from the standard curve in the ninth step;
step eleven, calculating the content of the harmful elements to be detected in the gold in the jewelry to be detected according to the following formula:
in the formula: omegaiThe content of harmful elements to be detected, mk/kg, contained in the gold in the jewelry to be detected;
Cistep ten, finding out the mass concentration of the harmful elements to be detected in the sample to be detected, ug/mL, from the standard curve;
v is the volume of the sample to be measured, mL;
m2weighing the mass of sample gold in the gold contained in the jewelry to be detected, namely mg.
The preparation method of the dilute nitric acid solution used in the third step and the fourth step of the invention comprises the following steps: 50mL of nitric acid with ρ 1.42g/mL was weighed and added to 150mL of secondary deionized water, followed by mixing.
In the fourth step of the invention, the concentration of the ammonium chloride solution is 20 g/L.
Example 1
The method is characterized in that 50mLN, N-dimethylacetamide reagent is added in the first step, the mixture is heated to boiling in an electric furnace plate and kept for 15min, the jewelry is uniformly cut into sections by using hydraulic tongs in the third step, the length of each section is 1cm, 50mL of dilute nitric acid solution is added, 30mL of ammonium chloride solution is added in the fourth step, the mixture is heated for 5min, the solution is poured out, the lower limit of the to-be-measured harmful element is determined to be 5mg/kg according to the sensitivity and detection limit of an instrument, and the quality of the pure silver gold-plated ring and the result of the to-be-measured harmful element are shown in table 1. The content of harmful elements is lower than the limit value specified in the ornament. TABLE 1 quality of gold and harmful elements in the gold-plated finger ring made of pure silver
| Mass m of gold in jewelry1 | Nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium, mercury |
| 0.2300g | Are all less than 5mg/kg |
Example 2
The method comprises the steps of measuring the pure silver gold-plated bracelet jewelry according to the method, wherein the difference is that 100mL of N, N-dimethylacetamide reagent is added in the first step, the bracelet jewelry is heated to boiling in an electric furnace disc and kept for 30min, the jewelry is uniformly cut into sections by using hydraulic tongs in the third step, the length of each section is 1.5cm, 100mL of dilute nitric acid solution is added, 50mL of ammonium chloride solution is added in the fourth step, the bracelet jewelry is heated for 10min, the solution is poured out, the lower limit of the to-be-measured harmful element is determined to be 5.0mg/kg according to the sensitivity and detection limit of an instrument, and the quality of gold in the pure silver gold-plated bracelet and the result of the measurement of the harmful element in the gold are shown in Table 2. The content of harmful elements is lower than the limit value specified in the ornament.
TABLE 2 gold quality and purity test data in gold-plated finger ring made of pure silver
| Mass m of gold in jewelry1 | Nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium, mercury |
| 0.9713g | Are all less than 5.0mg/kg |
Experimental example 1
At present, a standard sample of pure silver gold-plated jewelry does not exist, 25ug of standard substances of nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury, the theoretical contents of which are all 50mg/kg, are mixed into a pure silver gold-plated ring which is the same as that in the embodiment 1 to carry out a labeling test according to the method in the embodiment 1, the test result is shown in a table 3, and the recovery rate is 96.00-103.00%, which indicates that the method is accurate and reliable.
TABLE 3 test of recovery rate of harmful elements in gold-plated finger ring with silver
Experimental example 2
At present, a standard sample without pure silver gold-plated jewelry is taken, 50ug of standard substances of nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury, the theoretical contents of which are all 100mg/kg, are mixed into a pure silver gold-plated ring bracelet which is the same as that in the embodiment 2 to carry out a labeling test according to the method in the embodiment 2, the test result is shown in a table 4, and the recovery rate is between 98.50% and 101.5%, which indicates that the method is accurate and reliable.
TABLE 4 recovery rate test for harmful elements in gold-plated bracelet made of pure silver
Claims (3)
1. A method for measuring gold quality and harmful elements in gold of a pure silver gold-plated jewelry is characterized by comprising the following steps:
putting the jewelry to be tested into a 400mL beaker, adding 50 mL-100 mL of N, N-dimethylacetamide reagent, heating on an electric stove plate until boiling, and keeping for 15 min-30 min;
pouring out the solution in the beaker treated in the step one, washing the jewelry to be detected for 3-5 times by using secondary deionized water, and heating and drying the jewelry to be detected;
thirdly, shearing the jewelry to be detected into uniform sections by using hydraulic pliers, wherein the length of each section is 1-1.5 cm, putting the jewelry to be detected into a 400mL beaker, adding 50-100 mL of dilute nitric acid solution, and heating the jewelry to be detected on an electric stove plate at the temperature of 200 ℃ until no small bubbles are generated;
taking out gold by using plastic tweezers, washing the gold taken out for 3-5 times by using a dilute nitric acid solution, washing the gold taken out for 3-5 times by using water, putting the gold taken out into a 250mL beaker, adding 30-50 mL of ammonium chloride solution, heating for 5-10 min, pouring out the solution in the beaker, washing the gold in the beaker for 3-5 times by using water, and then putting the washed gold back into the 250mL beaker;
step five, adding 30mL of acetone into the 250mL beaker obtained in the step four, and putting the beaker into an ultrasonic machine for ultrasonic treatment for 10 min;
and step six, pouring out the solution in the beaker after the ultrasonic treatment is finished, placing the beaker in an electric oven at 100 ℃ for heating for 30min, taking out the beaker, cooling to room temperature, placing the gold in the beaker on an analytical balance for weighing, and recording the mass of the gold as m1The gold quality in the jewelry to be detected is obtained;
step seven, the mass obtained in the step six is m1Weighing mass m in gold2Placing 0.2000g of sample gold in a 25mL volumetric flask, adding 5mL of aqua regia, heating until the sample gold is completely dissolved, cooling, adding water to a constant volume to scale, and uniformly mixing, wherein the solution in the volumetric flask is a sample to be detected, and the volume is marked as V;
step eight, carrying out a blank test along with the sample;
weighing four parts of 0.2000g of high-purity gold, respectively placing the four parts of high-purity gold in four 25mL volumetric flasks, respectively adding 5mL of aqua regia into the four 25mL volumetric flasks, respectively heating until the high-purity gold in the volumetric flasks is completely dissolved, respectively adding standard solutions containing nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury into the four 25mL volumetric flasks so that the concentrations of the standard solutions containing nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury in each volumetric flask are respectively 0.00ug/mL, 1.00ug/mL, 2.00ug/mL and 4.00ug/mL, respectively measuring the spectral line intensities of nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury in the four 25mL volumetric flasks by using an inductively coupled plasma emission spectrometer, respectively measuring the mass concentrations of eleven elements of nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury in the four 25mL volumetric flasks as horizontal coordinates, the spectral line intensity is a standard curve drawn by a vertical coordinate;
step ten: measuring the spectral line intensity of eleven elements of nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury in the 25mL volumetric flask in the seventh step by using an inductively coupled plasma emission spectrometer, and finding out the mass concentration of the eleven elements of nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury to be tested in the seventh step from the standard curve in the ninth step;
step eleven, calculating the content of the harmful elements to be detected in the gold in the jewelry to be detected according to the following formula:
in the formula: omegaiThe content of harmful elements to be detected, mk/kg, contained in the gold in the jewelry to be detected;
Cistep ten, finding out the mass concentration of the harmful elements to be detected in the sample to be detected, ug/mL, from the standard curve;
v is the volume of the sample to be measured, mL;
m2weighing the mass of sample gold in the gold contained in the jewelry to be detected, namely mg.
2. The method for determining the gold quality and harmful elements in gold of the pure silver gold-plated jewelry according to claim 1, wherein the preparation method of the dilute nitric acid solution used in the third step and the fourth step is as follows: 50mL of nitric acid with ρ 1.42g/mL was weighed and added to 150mL of secondary deionized water, followed by mixing.
3. The method for determining the gold quality and harmful elements in gold of the pure silver gold-plated jewelry according to claim 1, wherein the concentration of the ammonium chloride solution in the step four is 20 g/L.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2061348C1 (en) * | 1995-09-06 | 1996-05-27 | Научно-производственное предприятие "Наука-Сервис" | METHOD FOR X-RAY FLUORESCENT DETERMINATION OF GOLD SAMPLES |
| JP2004028884A (en) * | 2002-06-27 | 2004-01-29 | Sumika Chemical Analysis Service Ltd | Quantitative analytical method for determining impurity element |
| CN102019282A (en) * | 2009-09-16 | 2011-04-20 | 中国科学院电子学研究所 | Method for purifying ceramic-metal structural component |
| US20110217564A1 (en) * | 2010-03-05 | 2011-09-08 | Suneeta Neogi | Method For Imparting Tarnish Protection Or Tarnish Protection With Color Appearance To Silver, Silver Alloys, Silver Films, Silver Products and Other Non Precious Metals |
| CN102279176A (en) * | 2011-08-19 | 2011-12-14 | 山东黄金矿业(莱州)有限公司精炼厂 | Simultaneous measuring method for impurity elements in silver |
| CN103019051A (en) * | 2012-12-07 | 2013-04-03 | 京东方科技集团股份有限公司 | Resist stripping solution |
| CN106018382A (en) * | 2016-05-17 | 2016-10-12 | 深圳市宁深检验检测技术有限公司 | Method for rapidly testing impurity elements in high-purity gold |
| CN106118213A (en) * | 2016-09-23 | 2016-11-16 | 重庆理工大学 | A kind of water-based plastic paint stripper and its preparation method and application |
| CN109234681A (en) * | 2018-09-25 | 2019-01-18 | 太仓弘潞新材料有限公司 | A method of preparing orderly gold nano cap array |
| CN110553887A (en) * | 2019-10-17 | 2019-12-10 | 北矿检测技术有限公司 | Method for quickly separating copper matrix for ICP-MS analysis of impurity elements in metal copper |
| CN110907527A (en) * | 2019-12-16 | 2020-03-24 | 重庆市计量质量检测研究院 | Method for measuring content of impurity elements in high-purity gold jewelry |
-
2020
- 2020-06-16 CN CN202010545768.2A patent/CN111650081B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2061348C1 (en) * | 1995-09-06 | 1996-05-27 | Научно-производственное предприятие "Наука-Сервис" | METHOD FOR X-RAY FLUORESCENT DETERMINATION OF GOLD SAMPLES |
| JP2004028884A (en) * | 2002-06-27 | 2004-01-29 | Sumika Chemical Analysis Service Ltd | Quantitative analytical method for determining impurity element |
| CN102019282A (en) * | 2009-09-16 | 2011-04-20 | 中国科学院电子学研究所 | Method for purifying ceramic-metal structural component |
| US20110217564A1 (en) * | 2010-03-05 | 2011-09-08 | Suneeta Neogi | Method For Imparting Tarnish Protection Or Tarnish Protection With Color Appearance To Silver, Silver Alloys, Silver Films, Silver Products and Other Non Precious Metals |
| CN102279176A (en) * | 2011-08-19 | 2011-12-14 | 山东黄金矿业(莱州)有限公司精炼厂 | Simultaneous measuring method for impurity elements in silver |
| CN103019051A (en) * | 2012-12-07 | 2013-04-03 | 京东方科技集团股份有限公司 | Resist stripping solution |
| CN106018382A (en) * | 2016-05-17 | 2016-10-12 | 深圳市宁深检验检测技术有限公司 | Method for rapidly testing impurity elements in high-purity gold |
| CN106118213A (en) * | 2016-09-23 | 2016-11-16 | 重庆理工大学 | A kind of water-based plastic paint stripper and its preparation method and application |
| CN109234681A (en) * | 2018-09-25 | 2019-01-18 | 太仓弘潞新材料有限公司 | A method of preparing orderly gold nano cap array |
| CN110553887A (en) * | 2019-10-17 | 2019-12-10 | 北矿检测技术有限公司 | Method for quickly separating copper matrix for ICP-MS analysis of impurity elements in metal copper |
| CN110907527A (en) * | 2019-12-16 | 2020-03-24 | 重庆市计量质量检测研究院 | Method for measuring content of impurity elements in high-purity gold jewelry |
Non-Patent Citations (10)
| Title |
|---|
| Y.C SUN: "Determination of trace impurities in high purity gold by inductively coupled plasma mass spectrometry with prior matrix removal by electrodeposition", 《SPECTROCHIMICA ACTA PART B: ATOMIC SPECTROSCOPY》 * |
| 中华人民共和国国家质量监督检验检疫总局: "《GB/T 21198.6-2007 贵金属合金首饰中贵金属含量的测定 ICP光谱法 第6部分：差减法》", 12 November 2007 * |
| 中华人民共和国国家质量监督检验检疫总局: "《GB/T 28016-2011 金合金首饰 金含量的测定 重量法》", 31 October 2011 * |
| 周西林等: "电感耦合等离子体原子发射光谱法在金属材料分析应用技术方面的进展", 《冶金分析》 * |
| 国家市场监督管理总局: "《GB/T 9288-2019 金合金首饰 金含量的测定 灰吹法（火试金法）》", 18 October 2019 * |
| 徐剑瑛: "电感耦合等离子体光谱法测定纯银中杂质元素", 《山东化工》 * |
| 戴永盛: "提高氯化银沉淀法回收银得率的探讨", 《电镀与精饰》 * |
| 林滔: "浅析铅火试金法铅的加入量", 《中国检验检测》 * |
| 马世昌: "《化学物质辞典》", 30 April 1999, 陕西科学技术出版社 * |
| 高孔: "EDX-LE型X射线能谱仪测试银饰品含量的条件设置", 《计量与测试技术》 * |
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