CN111650081B - 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
- Publication number
- CN111650081B CN111650081B CN202010545768.2A CN202010545768A CN111650081B CN 111650081 B CN111650081 B CN 111650081B CN 202010545768 A CN202010545768 A CN 202010545768A CN 111650081 B CN111650081 B CN 111650081B
- Authority
- CN
- China
- Prior art keywords
- gold
- jewelry
- detected
- beaker
- silver
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
Landscapes
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Immunology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Plasma & Fusion (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
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, acetone ultrasonic method solves the adhesion of impurity elements on the gold surface, and adopts ammonium chloride solution to stabilize 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 guaranteed value price of the jewelry, so that the accurate determination of the quality and purity of gold in jewelry is very important. 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 has the key problem of sample pretreatment that the coating layer on the surface of the jewelry can not be removed by adopting a proper method because the coating layer is firstly removed if the quality and the purity of gold need to be detected, the coating layer is organic matter and is tightly combined with the jewelry and can not be removed manually, and residues can be left on the surface of the jewelry by adopting a burning mode and can not be detected subsequently.
The quality of the precious metal jewelry is measured according to QB/T1690-2004 'Provisions on quality measurement tolerance of precious metal jewelry', the standard is suitable for precious metal detection of pure matrixes 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 micrometers, and the tested pure gold sample is required to have better uniformity and no sandwich and wrapping phenomena, so that the X-ray fluorescence spectrometry is not suitable for being used as an arbitration analysis method for precious metal jewelry samples.
As the precious metal jewelry is worn by people, the safety of the precious metal jewelry is more and more concerned by people, so that the content of harmful elements in the precious metal jewelry is checked, the market admission is strictly restricted, the influence of the harmful elements on the health of the human body is reduced or eliminated to the greatest extent, and the precious metal jewelry is the most important link in the precious metal jewelry check. 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 gold quality and the harmful elements in gold in pure silver gold-plating jewelry, which is particularly suitable for the pure silver gold-plating jewelry with the gold quality fraction not lower than 999 permillage.
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 jewelry to be tested on an electric furnace disc at the temperature of 200 ℃ until no small bubbles are generated;
step four, taking out gold by using a plastic forceps, washing the taken-out gold for 3-5 times by using a dilute nitric acid solution, washing the taken-out gold for 3-5 times by using water, putting the taken-out gold 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 putting the washed gold back into the 250mL beaker;
step five, adding 30mL of acetone into the 250mL beaker obtained in the step four, putting the beaker into an ultrasonic machine, and carrying out ultrasonic treatment for 10min;
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 m 1 The gold quality in the jewelry to be detected is obtained;
step seven, the mass obtained in the step six is m 1 The mass m of the gold is weighed 2 Placing 0.2000g of sample gold into 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 a 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 the four volumetric flasks 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, respectively, 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 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, and drawing a standard curve with the mass intensities of the spectral lines of eleven elements, namely nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury;
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: omega i The content of harmful elements to be detected contained in the gold in the jewelry to be detected is mg/kg;
C i step 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;
m 2 weighing the mass g of sample gold in gold contained in the jewelry to be detected.
The preparation method of the dilute nitric acid solution used in the third step and the fourth step comprises the following steps: a quantity of 50mL nitric acid with ρ =1.42g/mL was added to 150mL of secondary deionized water and mixed well.
In the fourth step, the concentration of the ammonium chloride solution is 20g/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 quickly determine the impurity elements in the pure gold, adopts the ammonium chloride solution to stabilize the complex silver ions, eliminates the influence of silver on the determination of the impurities, and fills the blank of determining the gold quality and the harmful elements in the gold of 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;
step four, taking out gold by using a plastic forceps, washing the taken-out gold by using a dilute nitric acid solution for 3-5 times, then washing the taken-out gold by using water for 3-5 times, putting the taken-out gold 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 by using water for 3-5 times, 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, putting the beaker into an ultrasonic machine, and carrying out ultrasonic treatment for 10min;
and step six, pouring out the solution in the beaker after the ultrasonic treatment is finished, placing the beaker in an electric oven at the temperature of 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 m 1 The 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 m 1 Weighing mass m in gold 2 Placing 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 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, and drawing a cross-line coordinate curve of the elements of the spectral line intensities of the nickel, bismuth, cadmium, cobalt, lead, antimony, arsenic, selenium and mercury;
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: omega i The content of harmful elements to be detected contained in the gold in the jewelry to be detected is mg/kg;
C i in the step ten, the mass concentration ug/mL of the harmful elements to be detected in the sample to be detected is found out from the standard curve;
v is the volume of the sample to be measured, mL;
m 2 weighing the mass g of sample gold in gold contained in the jewelry to be detected.
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 rho =1.42g/mL was weighed and added to 150mL of secondary deionized water, and the mixture was mixed well.
In the fourth step of the invention, the concentration of the ammonium chloride solution is 20g/L.
Example 1
The method is characterized in that 50mL of N, N-dimethylacetamide reagent is added in the first step, the mixture is heated to boiling in an electric stove 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 and poured out, the lower limit of the determination of the harmful elements to be determined is determined to be 5mg/kg according to the sensitivity and detection limit of an instrument, and the quality of the gold in the pure silver gold-plated ring and the determination result of the harmful elements in the gold 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 pure silver gold-plated finger ring
| Mass m of gold in jewelry 1 | Nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium, mercury |
| 0.2300g | Are all less than 5mg/kg |
Example 2
The bracelet jewelry plated with gold through pure silver is measured according to the method, wherein the difference is that 100mL of N, N-dimethylacetamide reagent is added in the first step, the bracelet 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 solution is heated for 10min and poured out, the lower limit of the harmful element to be measured is determined to be 5.0mg/kg according to the sensitivity and detection limit of an instrument, and the quality of gold in the bracelet plated with gold through pure silver and the result of the harmful element measurement are shown in a 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 jewelry 1 | Nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic,Selenium and 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, a standard sample of pure silver gold-plated jewelry, which is the same as that in the embodiment 1, is mixed with 25ug of each of nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury standard substances with theoretical content of 50mg/kg to carry out a standard adding test according to the method in the embodiment 1, the test result is shown in a table 3, the recovery rate is between 96.00% and 103.00%, and 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 (2)
1. A method for measuring the 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;
step four, taking out gold by using a plastic forceps, washing the taken-out gold for 3-5 times by using a dilute nitric acid solution, washing the taken-out gold for 3-5 times by using water, putting the taken-out gold 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 putting the washed gold back into the 250mL beaker;
wherein the concentration of the ammonium chloride solution is 20g/L;
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 10min;
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 m 1 The gold quality in the jewelry to be detected is obtained;
step seven, the mass obtained in the step six is m 1 Weighing mass m in gold 2 Placing 0.2000g of sample gold into 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 a 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 the four volumetric flasks 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, respectively, 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 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, and drawing a standard curve with the mass intensities of the spectral lines of eleven elements, namely nickel, bismuth, cadmium, cobalt, manganese, lead, chromium, antimony, arsenic, selenium and mercury;
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: omega i The content of harmful elements to be detected contained in gold in the jewelry to be detected is mg/kg;
C i in the step ten, the mass concentration ug/mL of the harmful elements to be detected in the sample to be detected is found out from the standard curve;
v is the volume of the sample to be measured, mL;
m 2 weighing the mass g of sample gold in gold contained in the jewelry to be detected.
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 rho =1.42g/mL was weighed and added to 150mL of secondary deionized water, and the mixture was mixed well.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010545768.2A CN111650081B (en) | 2020-06-16 | 2020-06-16 | Method for measuring gold quality and harmful elements in gold of pure-silver gold-plated jewelry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010545768.2A CN111650081B (en) | 2020-06-16 | 2020-06-16 | Method for measuring gold quality and harmful elements in gold of pure-silver gold-plated jewelry |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111650081A CN111650081A (en) | 2020-09-11 |
| CN111650081B true CN111650081B (en) | 2022-11-11 |
Family
ID=72344297
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010545768.2A Active CN111650081B (en) | 2020-06-16 | 2020-06-16 | Method for measuring gold quality and harmful elements in gold of pure-silver gold-plated jewelry |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111650081B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004028884A (en) * | 2002-06-27 | 2004-01-29 | Sumika Chemical Analysis Service Ltd | Quantitative analytical method for determining impurity element |
| 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 |
| 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 |
Family Cites Families (8)
| 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 |
| CN102019282B (en) * | 2009-09-16 | 2012-08-08 | 中国科学院电子学研究所 | Method for purifying ceramic-metal structural component |
| US8802202B2 (en) * | 2010-03-05 | 2014-08-12 | Suneeta S. 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 |
| CN103019051B (en) * | 2012-12-07 | 2015-11-25 | 京东方科技集团股份有限公司 | A kind of anticorrosive additive stripping liquid controlling |
| 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 |
-
2020
- 2020-06-16 CN CN202010545768.2A patent/CN111650081B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004028884A (en) * | 2002-06-27 | 2004-01-29 | Sumika Chemical Analysis Service Ltd | Quantitative analytical method for determining impurity element |
| 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 |
| 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 (5)
| Title |
|---|
| Determination of trace impurities in high purity gold by inductively coupled plasma mass spectrometry with prior matrix removal by electrodeposition;Y.C Sun;《Spectrochimica Acta Part B: Atomic Spectroscopy》;20000906;第55卷(第11期);1481-1489 * |
| EDX-LE型X射线能谱仪测试银饰品含量的条件设置;高孔;《计量与测试技术》;20150131;第42卷(第1期);1-3 * |
| 提高氯化银沉淀法回收银得率的探讨;戴永盛;《电镀与精饰》;19900930;第12卷(第5期);36-37 * |
| 浅析铅火试金法铅的加入量;林滔;《中国检验检测》;20170726(第4期);46-47,24 * |
| 电感耦合等离子体光谱法测定纯银中杂质元素;徐剑瑛;《山东化工》;20200131;第49卷(第1期);59-61 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111650081A (en) | 2020-09-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103412034A (en) | Measuring method for quickly measuring contents of heavy metals in tobacco by using microwave digestion/ICP-MS method | |
| Feng et al. | Determination of arsenic, antimony, selenium, tellurium and bismuth in nickel metal by hydride generation atomic fluorescence spectrometry | |
| CN113252645B (en) | Method for rapidly determining chromium content in copper or copper alloy | |
| Cheng et al. | Spectrophotometric determination of bismuth with sodium diethyldithiocarbamate | |
| CN105424462A (en) | Method of determining mercury in soil through water bath digestion-atomic fluorescence method | |
| CN109142664A (en) | The detection method of nickel element content in a kind of high iron-containing dilval | |
| CN111650081B (en) | Method for measuring gold quality and harmful elements in gold of pure-silver gold-plated jewelry | |
| CN106018382A (en) | Method for rapidly testing impurity elements in high-purity gold | |
| CN102243178A (en) | Rapid determination method for gold, silver, platinum and palladium in smelting wastewater of rare noble metals | |
| CN102928271A (en) | Sample treatment method for measuring niobium, tungsten and zirconium in steel | |
| Jotanović et al. | Comparison of x-ray fluorescent analysis and cupellation method for determination of gold in gold jewellery alloy | |
| CN105606414A (en) | A set of wire spectrum standard samples and preparation method | |
| CN107389664A (en) | The assay method of impurity content in a kind of high purity zinc | |
| Singh | A rugged, precise and accurate new gravimetry method for the determination of gold: an alternative to fire assay method | |
| de Jesus et al. | A separation method to overcome the interference of aluminium on zinc determination by inductively coupled plasma atomic emission spectroscopy | |
| CN104730010A (en) | Method for detecting content of lead in zinc alloy button | |
| Frank et al. | Spectrophotometric determination of copper in titanium | |
| CN115112520B (en) | Analysis method for gold content in cyanide-free hard gold | |
| Kayal et al. | Stepwise complexometric determination of aluminium, titanium and iron concentrations in silica sand and allied materials | |
| Gao et al. | ICP-OES determination of palladium in palladium jewellery alloys using Yttrium internal standard | |
| CN111999150B (en) | Method for measuring rhodium content in rhodium-ruthenium alloy | |
| CN114152489B (en) | Platinum-palladium-gold gray blowing method in black rock by taking tellurium-silver as protective agent | |
| Serih | A novel spectral method indirectly to estimate the lead in Cu-Zn-Pb bronze alloy | |
| Zhang et al. | Process optimization for the synthesis of functionalized Au@ AgNPs for specific detection of Hg 2+ based on quality by design (QbD) | |
| Li et al. | Determination of the concentration of prepared Rehmannia root solution by fluorescence polarization spectroscopy combined with the least-square method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |