QB/T 2382-1998 Test method for bright gold water and bright palladium gold water
Some standard content:
QB/T2382--1998
This standard is revised based on ZBY24005--1989 "Test Method for Bright Gold Water and Bright Palladium Gold Water". In recent years, through the opportunity of communication with foreign businessmen, we learned that there are only internal standards of enterprises abroad. With reference to these standards, most of the parts of this standard that have been proven to be suitable in practice have been retained, but some important technical indicators have been revised as follows: In the item "Gold and palladium determination" of bright palladium gold water, "move into a muffle furnace and burn at 700℃ for 20min" is changed to "move into a muffle furnace and burn at 800℃ for 15min". In the item "Testing of color firing temperature", "according to the method in Chapter 7", that is, painting the test piece according to the usual gold painting thickness, is changed to "painting two test pieces of standard area according to the method of 3.6" - In the item "Gold color test", "applying a gold water block of about 15cm" on clean porcelain or glass according to the usual thickness" is changed to "painting three porcelain or glass test pieces of standard area according to the method of 3.6". - GB/T5002-1985 "Method for Determination of Gold Water Precipitation Rate for Ceramics" is incorporated into this standard. From the date of implementation of this standard, it will replace ZBY24005--1989 "Test Method for Bright Gold Water and Bright Palladium Gold Water". This standard is proposed by the Quality Standards Department of China Light Industry Association. This standard is under the jurisdiction of the National Ceramic Standardization Center. The drafting unit of this standard: Hunan Ceramic Research Institute. The main drafters of this standard: Xiao Jiankun, Yi Yuehua, Wu Xianyi. 277
1 Scope
Light Industry Industry Standard of the People's Republic of China
Test Method for Bright Gold Water and Bright Palladium Gold Water
This standard specifies the test method for the technical indicators of bright gold water and bright palladium gold water. This standard is applicable to bright gold water and bright palladium gold water used for decoration of porcelain, ceramics, fine pottery and glass products. 2 Referenced Standards
QB/T2382-1998
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are all valid. All standards are subject to revision. Parties using this standard should explore the possibility of using the latest versions of the following standards: GB/T5000-1985 Terminology of ceramics for use in the catalog QB/T2381--1998 Bright gold water Bright palladium gold water 3 Determination method
3.1 Property inspection
Inspect by visual inspection, observe the color by smear, and the dark color is qualified. 3.2 Net weight inspection
3.2.1 Instrument
Use a rack pharmaceutical balance or analytical balance with a sensitivity of 0.1g. 3.2.2 Steps
Remove the seal of the gold water sample bottle, leaving the inner stopper, and weigh it on a rack balance, and record the mass value W (g), accurate to 0.1. Then transfer all the gold water in the bottle to another clean empty bottle, rinse out the remaining gold water in the bottle with chloroform, wipe off the oil in the bottle and on the bottle stopper with dry filter paper, and then weigh the mass value W. (g) of the empty bottle and the bottle stopper, and calculate the mass of the gold water W () according to formula (1). W.-- W, -- W.
W. Mass of bottled gold water Name:
W Mass of empty bottle and bottle stopper?
3.3 Determination of gold content
3.3.1 Determination of gold content in bright gold water
3.3.1.1 Principle
Burn the gold water to remove organic matter, melt the residue with potassium pyrosulfate and treat it with dilute nitric acid to remove impurities, burn the pure gold residue and weigh it. 3.3.1.2 Reagents
Potassium pyrosulfate, AR
Nitric acid, AR;
Monofluoride, AR;
One absorbent cotton (medical use).
3.3.1.3 Instruments
Approved by the State Bureau of Light Industry on 1998-05-14
1999-03-01. Bottle
Ceramic crucible: 50mL;
Beaker: 250mL:
—Funnel,
One medium-speed quantitative filter paper:
One muffle furnace;
Analytical balance (division value 0.1mg).
3.3.1.4 Steps
QB/T 2382—1998
Shake the sample bottle thoroughly until there is no sediment at the bottom of the bottle. Immediately weigh 1.5~2g of bright gold water by the reduction method using an analytical balance + deduction to 0.0001g. Place it in a 50ml porcelain crucible with constant weight. The crucible is pre-padded with about 1.5g of absorbent cotton so that the gold water is completely absorbed in the cotton ball. Place the crucible on the electric furnace plate to slowly carbonize, then move it to a muffle furnace and burn it at 700C until it is completely carbonized, about 20min. Take it out and cool it, add 6g of potassium pyrosulfate, cover the crucible, put it back in the muffle furnace, and melt it at 600C for 20min. Cool, extract the molten block with hot water in a 250mL beaker, clean the crucible and cover, add nitric acid that is one-third of the volume of the solution and boil, cool slightly, filter with medium-speed filter paper, wash several times with 1:3 dilute nitric acid, and then wash with hot water until there is no sulfate (check with 10% barium chloride solution that there is no white precipitate in the filtrate). Put the filter paper and the gold slag back into the original crucible, first carbonize at low temperature, then burn in a muffle furnace at 800C for 10 minutes, take out and put into a desiccator to keep for 40 minutes. until constant weight, weigh. 3.3.1.5 Calculation
A,(%) = (WI/G,) X 100
W-gold mass·.
G…-sample mass·g.
Parallel determination deviation is not more than 0.04%.
3.3.2 Determination of gold content in bright palladium water
...( 2)
3.3.2.1 Principle
Burning bright palladium water to remove organic matter, reducing palladium oxide to metallic palladium with sodium formate, dissolving gold and palladium with aqua regia, filtering and separating insoluble matter, reducing gold chloride to gold with sodium nitrite, filtering out gold precipitate, calcining and weighing. 3.3.2.2 Reagents
Sodium formate, AR,
Hydrochloric acid, AR (1% solution);
Nitric acid, AR;
-Sodium nitrite, AR (15% solution);
-Silver nitrate, AR (1% solution).
3.3.2.3 Apparatus and supplies
Universal test paper: pH1～12:
Absorbent cotton;
Ceramic crucible: 50ml.;
---Beaker: 250ml.
A slow filter paper
--Analytical balance (division value 0.1mg);
Muffle furnace;
-Dryer.
3.3.2.4 Steps
Shake the sample thoroughly until there is no sediment at the bottom of the bottle. Immediately weigh about 3g of the bright palladium gold water sample using the reduction method with an analytical balance and place it in a 50mL ceramic crucible with about 1.5g of absorbent cotton in advance. First, carbonize at low temperature, then move into a boiling furnace, burn at 279
QB/T 2382-- 1998
800C for 15min. Cool, and pour all the burnt materials into a 250mL beaker. Rinse with 3-4mL water to moisten the gold ash, add 0.3g formic acid, cover the surface, and heat to a slight boil for 2min. Then add 15mL acid and 5ml caustic soda to the cup, heat to dissolve, and concentrate to about 3mL, take out the surface III, move the cup to a boiling water bath and heat, concentrate to nearly dry, add 4mL hydrochloric acid, evaporate to 1.5mL, and repeat the hydrochloric acid operation once. Take out the beaker and dilute the gold solution with warm water until a white precipitate of hydrolyzate is produced. Filter while hot. Wash the paint cup and filter paper with warm water several times until the paper is colorless. Heat the filtrate to near boiling, and under stirring, add 15% sodium nitrite solution to reduce gold until the pH reaches 5 (add a small piece of test paper produced by the factory, and observe immediately after boiling). Boil for 2 minutes, cool, filter the gold precipitate with filter paper, wash the cup and filter paper with warm water 5-6 times (move the filtrate aside for palladium testing), and continue to wash the filter paper with warm water until there is no chloride ion (check with 1% silver nitrate). Wipe the gold in the cup with a small piece of filter paper, put the paper and gold into a weighed crucible, and after low carbonization, place it in a muffle furnace, burn at 800℃ for 10 minutes, cool, move to a desiccator and keep for 40 minutes, and weigh it. 3.3.2.5 Calculation
A2(%) m (W2/G) X 100
W Where: Gold content
W.--gold mass.g+
G sample mass g.
Parallel determination deviation is not greater than 0.%.
3.3.3 Determination of palladium content in palladium-gold water
33.3.1 Principle
The filtrate filtered from the gold precipitate in 3.3.2.4 is boiled with hydrochloric acid to destroy the palladium nitrite complex, so that the complex palladium is converted into chloropalladium salt, and then precipitated into diacetyl palladium with diacetyl, filtered, dried and weighed. 3.3.3.2 Reagents
Hydrochloric acid.AR:
T diacetyl AR;
-absolute alcohol
3.3.3.3 Instruments and supplies
1.4 glass sand core 30mL:
Filter:
Drying machine:
Analytical balance (division 0.1mg).
3. 3.3.4 Steps
Add 7mL hydrochloric acid to the lead solution left in 3.3.2.4 and heat to boil for 5min. After cooling to low temperature, add 35mL 1% triacetin alcohol solution and stir slowly, let stand for 1h, filter with dried constant weight No. 4 glass sand core, wash the cup and precipitate with 109mL 1% hydrochloric acid solution, and then wash once with 100mL water. Place the glass crucible in a box and dry at 110℃ for 1h to cool, move to a dryer and keep at 40 min, weigh
3.3.3.5 Calculate
B(%)0.3161x(WW/GX100
Wu Zhong: Palladium content:
W Wa and palladium precipitate mass.g
. Empty sweet glass mass area
G Sample mass g
0.3161 Conversion factor of palladium precipitate.
Parallel determination deviation is not more than 0.04%.
3.4 Determination of kinematic viscosity
First use a liquid with known kinematic viscosity (cyclohexanone at 30°C has a kinematic viscosity of 361×10~m3/s) in an Ostwald viscometer (capillary 280
QB/T 2382---1998
Inner diameter of the tube is 1.5mm. Tide is 30°C ± 0.5°C). The outflow time is measured. According to formula (5), the viscometer constant is obtained, point = /t
Wu Zhong: U.S. viscometer constant, m/s
-kinematic viscosity of the liquid with known kinematic viscosity, m*/s; the flow time of the body with known kinematic viscosity, then replace the liquid with known kinematic viscosity with gold water, measure the outflow time, and calculate the kinematic viscosity of gold water according to formula (6). Wa=g xt
In the formula; y2\-kinematic viscosity of gold water, m\/s-viscometer constant 22s*
-outflow time of gold water, S.
3.5 Photographic performance test
...--( 6 )
Use a gold-drawing pen to dip a proper amount of gold water sample, and draw different thick and thin lines and cross lines on a clean and dry porcelain piece according to the usual gold-drawing thickness to understand whether the gold water drawing is smooth or sluggish. Leave it for a few minutes, and observe whether the lines maintain the original width or widen, and whether the cross-line corners are gradually clear or rounded.
3.6 Determination of brushing area
Put more than 23 gold water in a clean small glass bottle, and insert a brush (the pen holder can be cut short for easy operation). After weighing the mass, take out the pen with gold water, and draw a rectangular block roughly equal to 3cm×5cm on the porcelain or glass test piece. The thickness of the entire coating should be uniform. After painting, put the pen back to the original bottle and weigh it again. The difference between the two masses is the amount of gold water consumed G. Use a ruler to measure the length and width of the coating defect (accurate to 0.1cm) and calculate the area S. The ratio of S to G is the coating area. If the batch value does not match the specified value, it is necessary to re-coat the piece according to the method until it meets the requirements.
37 Drying speed determination
Use a gold-drawing pen to dip a proper amount of gold water sample, and on a clean and dry porcelain piece, draw 20 thick and thin parallel lines or cross lines with different thicknesses on the surface according to the usual gold-drawing thickness. After the completion, record the time, put the test piece at room temperature of about 25℃ or in a constant temperature box, and gently touch the gold line with your finger every 10 minutes. When the gold line of medium thickness does not stick to your finger, record the time. The difference between the two times is the drying speed. 3.8 Color firing degree inspection
Apply two test pieces of standard area according to the method in 3.6, and color-fire at the upper and lower limits of the color-fired temperature respectively. Color firing method: Place one of the test pieces in the center of the muffle furnace, below the tip of the thermocouple, and use a refractory rack to support the test piece so that it is 1 cm above the furnace bottom. Close the furnace door and turn on the power to heat it. Before 400°C, a small gap should be left in the furnace door to exhaust smoke. After 400°C, close the furnace door tightly and burn it to the lower limit temperature specified in this standard. Keep it for 15 minutes and then turn off the power. Cool it with the half-open furnace door and take out the test piece. Heat the other test piece to the upper limit temperature in the same way, keep it at the upper limit temperature for 10 minutes, cool it, and take out the test piece.
Check the adhesion of the gold layer of the test pieces at each temperature, and check whether the test piece burned to the upper limit temperature has discoloration. The one with strong adhesion and no discoloration is qualified.
3.9 Gold burning test
Coat three porcelain or glass test pieces according to the method in 3.6, and place them in the muffle furnace to burn within the range of this standard. Observe the gold blocks made. The gold should be bright and free of contamination and other colors. Measure at a distance of 50mm. Only one circular spot with a diameter of no more than 0.3mm is allowed on the three blocks, except for the spots (non-circular) caused by impurities brought in due to lax operation. Note: For new brushes with glue, the glue should be filtered and washed with water before use, and then dried. 3.10 Adhesion Test
3.10.1 Instruments and Materials
JMY Gold Abrasion Tester:
50mm×50mm smooth glazed flat porcelain pieces: -50mm×50mmx3mm flat window glass pieces -pure cotton cloth, boil with water to remove the glue, dry and cut into 10 pieces of 32mm round shape, and store in a safe place. 281
3.10.2 Steps
QB/T 2382—1998
According to method 3.6, apply gold water to two standard push-up blocks, sinter within the standard range, keep warm for 15 minutes, take out the test piece and place it indoors for about 4 hours, then fix it on the gold abrasion tester sample table. Put five layers of cotton cloth on the grinding head and conduct a counting friction test. For porcelain and pond porcelain, gold water is used, and a 500g magnetic code is placed on the grinding head in advance, and reciprocating friction is performed 100 times: for glass and fine pottery, gold water is used, and no magnetic code is added to the grinding head (the grinding head itself is 65g), and reciprocating friction is performed 10 times. Two test pieces are required for each gold water, and the outer cloth piece on the grinding head must be replaced before each test piece is measured. If the results of the two test pieces are inconsistent, a third test piece must be measured, and the two closest test pieces are taken as the final results. 3.10.3 Result judgment
Observe the friction center, if there is no gold removal and bottom exposure phenomenon, it is qualified. 3.11 Determination of precipitation rate
3.11.1 Reagents
-Cyclohexanone, AR. www.bzxz.net
3.11.2 Instruments
Analytical balance, graduation value 0.1mg,
Constant temperature drying oven, the highest temperature is not less than 200℃; centrifugal sedimentation machine, the speed is not less than 2500t/min flat weighing bottle, 5cm.
3.11.3 Determination steps
Take a piece of slow quantitative filter paper, fold it and put it in the weighing bottle, open the bottle mouth and dry it in a constant temperature drying oven at 105-110℃ for 1h, cover the bottle cap, move it to a dryer to cool for 40min and weigh it, repeat the operation until constant weight (W,). Then take the prepared gold water sample, shake it thoroughly to make the precipitate not adhere to the bottom of the bottle, and then transfer it all to the filter paper with constant weight for filtration (when filtering, the liquid level should not exceed half the height of the filter paper, the same below), and wash it with a small amount of cyclohexanone once or twice. The filtrate is used to receive the clean beaker and transferred to the original filter paper for filtration again. The gold water bottle and beaker are cleaned with cyclohexanone, and the obtained washing liquid is transferred to the filter paper for filtration. Finally, the gold water on the filter paper is washed with cyclohexanone until the washing liquid is colorless. Fold the filter paper with the precipitate and place it in the original weighing bottle, open the bottle mouth and dry it in a constant temperature drying oven at 105-110℃ for 1h. Cover the bottle cap and move it into the dryer to cool for 40 minutes, take it out, weigh it, and repeat the operation until the constant weight (W). The precipitation rate of gold water T(%) is calculated according to formula (7): T(%) = (W - W)/GX 100
Wt—the mass of filter paper and weighing bottle before filtration, g; WL—the mass of filter paper and weighing bottle after filtration + g, G—the net mass of the whole bottle of gold water, nom.
The deviation of parallel determination shall not exceed 0.04%.
3.12 Hiding power test
Only glass gold water is tested.
Under the gold layer thickness of the standard brushing area (see 3.6), at a distance of 50cm, look directly at the light, and visually inspect the fired test piece. If there is no obvious light transmission phenomenon, it is qualified.3161x(WW/GX100
Wu Zhong: Palladium content:
W Wa and palladium precipitation mass.g
. Empty sweet glass mass area
G Sample mass g
0.3161 Conversion factor of palladium precipitation.
Parallel determination deviation is not more than 0.04%.
3.4 Determination of kinematic viscosity
First, use a liquid with known kinematic viscosity (cyclohexanone at 30°C has a kinematic viscosity of 361×10~m3/s) in an Ostwald viscometer (capillary 280
QB/T 2382---1998
Inner diameter of the tube is 1.5mm. Tide is 30°C ± 0.5°C). The outflow time is measured. According to formula (5), the viscometer constant is obtained, point = /t
Wu Zhong: U.S. viscometer constant, m/s
-kinematic viscosity of the liquid with known kinematic viscosity, m*/s; the flow time of the body with known kinematic viscosity, then replace the liquid with known kinematic viscosity with gold water, measure the outflow time, and calculate the kinematic viscosity of gold water according to formula (6). Wa=g xt
In the formula; y2\-kinematic viscosity of gold water, m\/s-viscometer constant 22s*
-outflow time of gold water, S.
3.5 Photographic performance test
...--( 6 )
Use a gold-drawing pen to dip a proper amount of gold-water sample, and draw different thick and thin lines and cross lines on a clean and dry porcelain piece according to the usual gold-drawing thickness to understand whether the gold-water drawing is smooth or sluggish. Leave it for a few minutes, and observe whether the lines maintain their original width or widen, and whether the cross-line corners are gradually clear or rounded.
3.6 Determination of brushing area
Put more than 23 gold water in a clean small glass bottle, insert a brush (the pen holder can be cut short) , easy to operate). After weighing the mass, take out the pen with gold water and draw a rectangular block roughly equal to 3cm×5cm on the porcelain or glass test piece. The coating thickness of the whole piece should be uniform. After drawing, put the pen back to the original bottle and weigh the mass again. The difference between the two masses is the amount of gold water consumed G. Use a ruler to measure the length and width of the coating gap (accurate to 0.1cm) and calculate the area S. The ratio of S to G is the coating area. If the batch value does not meet the specified value, it is necessary to re-coat the piece according to the method until it meets the requirements.
37 Drying speed determination
Use a gold-drawing pen to dip a proper amount of gold water sample, and draw 20 parallel lines or cross lines of different thicknesses and thicknesses on a clean and dry porcelain piece according to the usual gold-drawing thickness. After the completion, record the time, place the test piece at room temperature of about 25℃ or in a constant temperature box, and gently touch the gold line with your finger every 10 minutes. When the gold line of medium thickness does not stick to your finger, record the time. The difference between the two times is the drying speed. 3.8 Color firing degree inspection| |tt||Apply the two test pieces of standard area according to the method in 3.6, and respectively apply the test pieces at the upper and lower limits of the color firing temperature. Color firing method: Place one of the test pieces in the center of the muffle furnace, below the tip of the thermocouple, and use a refractory rack to support the test piece so that it is ? cm above the furnace bottom. Close the furnace door, turn on the power to heat it. Before 400℃, a small gap should be left in the furnace door to exhaust smoke. After 400℃, close the furnace door tightly and continue to heat it to the lower limit temperature specified in this standard. Keep it for 15 minutes and then turn off the power. Cool it with the furnace door half open, and take out the test piece. Heat the other test piece to the upper limit temperature according to the same method, keep it at the upper limit temperature for 10 minutes, cool it, and take out the test piece.
Check the adhesion of the gold layer of the test pieces at each temperature, and check whether the test piece burned to the upper limit temperature has discoloration. The one with strong adhesion and no discoloration is qualified.
3.9 Gold burning test
Apply three porcelain or glass test pieces according to the method in 3.6, and place them in a muffle furnace and burn them within the range of this standard. Observe the gold blocks made. The gold should be bright and free of contamination and variegated colors. Measure at a distance of 50mm. Only one circular spot with a diameter not greater than 0.3mm is allowed on the three blocks, except for spots (non-circular) caused by impurities brought in due to lax operation. Note: For new brushes with glue, they should be filtered with water in advance and the glue should be washed and dried before use. 3.10 Adhesion test
3.10.1 Instruments and materials
JMY gold abrasion tester:
Several pieces of 50mm×50mm glazed flat porcelain pieces: -Several pieces of 50mm×50mmx3mm flat window glass -Pure cotton cloth, pre-boil with water and wash to remove the glue. After drying, cut into 10 pieces of 32mm round shape and store in a safe place. 281
3.10.2 Steps
QB/T 2382—1998
According to method 3.6, apply gold water to two standard push-up blocks, sinter within the standard range, keep warm for 15 minutes, take out the test piece and place it indoors for about 4 hours, then fix it on the gold abrasion tester sample table. Put five layers of cotton cloth on the grinding head and conduct a counting friction test. For porcelain and pond porcelain, gold water is used, and a 500g magnetic code is placed on the grinding head in advance, and reciprocating friction is performed 100 times: for glass and fine pottery, gold water is used, and no magnetic code is added to the grinding head (the grinding head itself is 65g), and reciprocating friction is performed 10 times. Two test pieces are required for each gold water, and the outer cloth piece on the grinding head must be replaced before each test piece is measured. If the results of the two test pieces are inconsistent, a third test piece must be measured, and the two closest test pieces are taken as the final results. 3.10.3 Result judgment
Observe the friction center, if there is no gold removal and bottom exposure phenomenon, it is qualified. 3.11 Determination of precipitation rate
3.11.1 Reagents
-Cyclohexanone, AR.
3.11.2 Instruments
Analytical balance, graduation value 0.1mg,
Constant temperature drying oven, the highest temperature is not less than 200℃; centrifugal sedimentation machine, the speed is not less than 2500t/min flat weighing bottle, 5cm.
3.11.3 Determination steps
Take a piece of slow quantitative filter paper, fold it and put it in the weighing bottle, open the bottle mouth and dry it in a constant temperature drying oven at 105-110℃ for 1h, cover the bottle cap, move it to a dryer to cool for 40min and weigh it, repeat the operation until constant weight (W,). Then take the prepared gold water sample, shake it thoroughly to make the precipitate not adhere to the bottom of the bottle, and then transfer it all to the filter paper with constant weight for filtration (when filtering, the liquid level should not exceed half the height of the filter paper, the same below), and wash it with a small amount of cyclohexanone once or twice. The filtrate is used to receive the clean beaker and transferred to the original filter paper for filtration again. The gold water bottle and beaker are cleaned with cyclohexanone, and the obtained washing liquid is transferred to the filter paper for filtration. Finally, the gold water on the filter paper is washed with cyclohexanone until the washing liquid is colorless. Fold the filter paper with the precipitate and place it in the original weighing bottle, open the bottle mouth and dry it in a constant temperature drying oven at 105-110℃ for 1h. Cover the bottle cap and move it into the dryer to cool for 40 minutes, take it out, weigh it, and repeat the operation until the constant weight (W). The precipitation rate of gold water T(%) is calculated according to formula (7): T(%) = (W - W)/GX 100
Wt—the mass of filter paper and weighing bottle before filtration, g; WL—the mass of filter paper and weighing bottle after filtration + g, G—the net mass of the whole bottle of gold water, nom.
The deviation of parallel determination shall not exceed 0.04%.
3.12 Hiding power test
Only glass gold water is tested.
Under the gold layer thickness of the standard brushing area (see 3.6), at a distance of 50cm, look directly at the light, and visually inspect the fired test piece. If there is no obvious light transmission phenomenon, it is qualified.3161x(WW/GX100
Wu Zhong: Palladium content:
W Wa and palladium precipitation mass.g
. Empty sweet glass mass area
G Sample mass g
0.3161 Conversion factor of palladium precipitation.
Parallel determination deviation is not more than 0.04%.
3.4 Determination of kinematic viscosity
First, use a liquid with known kinematic viscosity (cyclohexanone at 30°C has a kinematic viscosity of 361×10~m3/s) in an Ostwald viscometer (capillary 280
QB/T 2382---1998
Inner diameter of the tube is 1.5mm. Tide is 30°C ± 0.5°C). The outflow time is measured. According to formula (5), the viscometer constant is obtained, point = /t
Wu Zhong: U.S. viscometer constant, m/s
-kinematic viscosity of the liquid with known kinematic viscosity, m*/s; the flow time of the body with known kinematic viscosity, then replace the liquid with known kinematic viscosity with gold water, measure the outflow time, and calculate the kinematic viscosity of gold water according to formula (6). Wa=g xt
In the formula; y2\-kinematic viscosity of gold water, m\/s-viscometer constant 22s*
-outflow time of gold water, S.
3.5 Photographic performance test
...--( 6 )
Use a gold-drawing pen to dip a proper amount of gold-water sample, and draw different thick and thin lines and cross lines on a clean and dry porcelain piece according to the usual gold-drawing thickness to understand whether the gold-water drawing is smooth or sluggish. Leave it for a few minutes, and observe whether the lines maintain their original width or widen, and whether the cross-line corners are gradually clear or rounded.
3.6 Determination of brushing area
Put more than 23 gold water in a clean small glass bottle, insert a brush (the pen holder can be cut short) , easy to operate). After weighing the mass, take out the pen with gold water and draw a rectangular block roughly equal to 3cm×5cm on the porcelain or glass test piece. The coating thickness of the whole piece should be uniform. After drawing, put the pen back to the original bottle and weigh the mass again. The difference between the two masses is the amount of gold water consumed G. Use a ruler to measure the length and width of the coating gap (accurate to 0.1cm) and calculate the area S. The ratio of S to G is the coating area. If the batch value does not meet the specified value, it is necessary to re-coat the piece according to the method until it meets the requirements.
37 Drying speed determination
Use a gold-drawing pen to dip a proper amount of gold water sample, and draw 20 parallel lines or cross lines of different thicknesses and thicknesses on a clean and dry porcelain piece according to the usual gold-drawing thickness. After the completion, record the time, place the test piece at room temperature of about 25℃ or in a constant temperature box, and gently touch the gold line with your finger every 10 minutes. When the gold line of medium thickness does not stick to your finger, record the time. The difference between the two times is the drying speed. 3.8 Color firing degree inspection| |tt||Apply the two test pieces of standard area according to the method in 3.6, and respectively apply the test pieces at the upper and lower limits of the color firing temperature. Color firing method: Place one of the test pieces in the center of the muffle furnace, below the tip of the thermocouple, and use a refractory rack to support the test piece so that it is ? cm above the furnace bottom. Close the furnace door, turn on the power to heat it. Before 400℃, a small gap should be left in the furnace door to exhaust smoke. After 400℃, close the furnace door tightly and continue to heat it to the lower limit temperature specified in this standard. Keep it for 15 minutes and then turn off the power. Cool it with the furnace door half open, and take out the test piece. Heat the other test piece to the upper limit temperature according to the same method, keep it at the upper limit temperature for 10 minutes, cool it, and take out the test piece.
Check the adhesion of the gold layer of the test pieces at each temperature, and check whether the test piece burned to the upper limit temperature has discoloration. The one with strong adhesion and no discoloration is qualified.
3.9 Gold burning test
Apply three porcelain or glass test pieces according to the method in 3.6, and place them in a muffle furnace and burn them within the range of this standard. Observe the gold blocks made. The gold should be bright and free of contamination and variegated colors. Measure at a distance of 50mm. Only one circular spot with a diameter not greater than 0.3mm is allowed on the three blocks, except for spots (non-circular) caused by impurities brought in due to lax operation. Note: For new brushes with glue, they should be filtered with water in advance and the glue should be washed and dried before use. 3.10 Adhesion test
3.10.1 Instruments and materials
JMY gold abrasion tester:
Several pieces of 50mm×50mm glazed flat porcelain pieces: -Several pieces of 50mm×50mmx3mm flat window glass -Pure cotton cloth, pre-boil with water and wash to remove the glue. After drying, cut into 10 pieces of 32mm round shape and store in a safe place. 281
3.10.2 Steps
QB/T 2382—1998
According to method 3.6, apply gold water to two standard push-up blocks, sinter within the standard range, keep warm for 15 minutes, take out the test piece and place it indoors for about 4 hours, then fix it on the gold abrasion tester sample table. Put five layers of cotton cloth on the grinding head and conduct a counting friction test. For porcelain and pond porcelain, gold water is used, and a 500g magnetic code is placed on the grinding head in advance, and reciprocating friction is performed 100 times: for glass and fine pottery, gold water is used, and no magnetic code is added to the grinding head (the grinding head itself is 65g), and reciprocating friction is performed 10 times. Two test pieces are required for each gold water, and the outer cloth piece on the grinding head must be replaced before each test piece is measured. If the results of the two test pieces are inconsistent, a third test piece must be measured, and the two closest test pieces are taken as the final results. 3.10.3 Result judgment
Observe the friction center, if there is no gold removal and bottom exposure phenomenon, it is qualified. 3.11 Determination of precipitation rate
3.11.1 Reagents
-Cyclohexanone, AR.
3.11.2 Instruments
Analytical balance, graduation value 0.1mg,
Constant temperature drying oven, the highest temperature is not less than 200℃; centrifugal sedimentation machine, the speed is not less than 2500t/min flat weighing bottle, 5cm.
3.11.3 Determination steps
Take a piece of slow quantitative filter paper, fold it and put it in the weighing bottle, open the bottle mouth and dry it in a constant temperature drying oven at 105-110℃ for 1h, cover the bottle cap, move it to a dryer to cool for 40min and weigh it, repeat the operation until constant weight (W,). Then take the prepared gold water sample, shake it thoroughly to make the precipitate not adhere to the bottom of the bottle, and then transfer it all to the filter paper with constant weight for filtration (when filtering, the liquid level should not exceed half the height of the filter paper, the same below), and wash it with a small amount of cyclohexanone once or twice. The filtrate is used to receive the clean beaker and transferred to the original filter paper for filtration again. The gold water bottle and beaker are cleaned with cyclohexanone, and the obtained washing liquid is transferred to the filter paper for filtration. Finally, the gold water on the filter paper is washed with cyclohexanone until the washing liquid is colorless. Fold the filter paper with the precipitate and place it in the original weighing bottle, open the bottle mouth and dry it in a constant temperature drying oven at 105-110℃ for 1h. Cover the bottle cap and move it into the dryer to cool for 40 minutes, take it out, weigh it, and repeat the operation until the constant weight (W). The precipitation rate of gold water T(%) is calculated according to formula (7): T(%) = (W - W)/GX 100
Wt—the mass of filter paper and weighing bottle before filtration, g; WL—the mass of filter paper and weighing bottle after filtration + g, G—the net mass of the whole bottle of gold water, nom.
The deviation of parallel determination shall not exceed 0.04%.
3.12 Hiding power test
Only glass gold water is tested.
Under the gold layer thickness of the standard brushing area (see 3.6), at a distance of 50cm, look directly at the light, and visually inspect the fired test piece. If there is no obvious light transmission phenomenon, it is qualified.6 Determination of coated area
Put more than 23gold water in a clean small glass bottle and insert a brush (the pen holder can be cut short for easy operation). After weighing the mass, take out the brush with gold water and draw a rectangular block roughly equal to 3cm×5cm on the porcelain or glass test piece. The coating thickness of the whole piece should be uniform. After drawing, put the pen back to the original bottle and weigh the mass again. The difference between the two masses is the amount of gold water consumed G. Use a ruler to measure the length and width of the coating gap (accurate to 0.1cm) and calculate the area S. The ratio of S to G is the coating area. If the batch value does not meet the specified value, it is necessary to re-coat the piece according to the method until it meets the requirements.
37 Determination of drying speed
Use a gold drawing pen to dip an appropriate amount of gold water sample, and draw 20 thick and thin parallel lines or cross lines with different thickness on the clean and dry porcelain piece according to the usual gold drawing thickness. After the test, record the time, place the test piece at room temperature of about 25℃ or in a constant temperature box, and gently touch the gold wire with your finger every 10 minutes. When the gold wire of medium thickness does not stick to your finger, record the time. The difference between the two times is the drying speed. 3.8 Color firing temperature test
Apply two test pieces of standard area according to the method in 3.6, and fire at the upper and lower limits of the color firing temperature respectively. Color firing method: Place one of the test pieces in the center of the muffle furnace, below the tip of the thermocouple, and use a refractory rack to support the test piece so that it is ? cm high from the bottom of the furnace. Close the furnace door, turn on the power to heat it. Before 400℃, the furnace door should leave a small gap to exhaust smoke. After 400℃, close the furnace door tightly and burn it to the lower limit temperature specified in this standard. Keep it for 15 minutes and then turn off the power. Cool it with the furnace door half open, and take out the test piece. Heat the other test piece to the upper limit temperature according to the same method, keep it at the upper limit temperature for 10 minutes, cool it, and take out the test piece.
Check the adhesion of the gold layer of the test pieces at each temperature, and check whether the test pieces burned to the upper limit temperature have discoloration. The test pieces with strong adhesion and no discoloration are qualified.
3.9 Gold burning test
Apply three porcelain or glass test pieces according to the method in 3.6, and place them in a muffle furnace to burn within the range of this standard. Observe the gold blocks made. The gold should be bright and free of contamination and other colors. When measured at a distance of 50mm, the three blocks are allowed to have only one circular spot with a diameter not greater than 0.3mm, except for spots (non-circular) caused by impurities brought in due to lax operation. Note: For new brushes that are glued, they should be filtered with water and cleaned of adhesives before use, and then dried. 3.10 Adhesion test
3.10.1 Instruments and materials
JMY gold abrasion tester:
50mm×50mm smooth glazed flat porcelain pieces: -50mm×50mmx3mm flat window glass pieces -Pure cotton cloth, pre-boil with water and rub to remove the glue. After drying, cut into 10 pieces of 32mm round shape, and store in a safe place. 281
3.10.2 Steps
QB/T 2382—1998
Apply gold water to two pieces of standard push area according to the method in 3.6, fire within the standard range, keep warm for 15 minutes, take out the test piece and place it in the room for about 4 hours, and then fix it on the gold abrasion tester sample table. Place five layers of cotton cloth on the grinding head and conduct a counting friction test. For porcelain and pond porcelain, use gold water, place a 500g magnetic code on the grinding head in advance, and rub back and forth 100 times: for glass and fine pottery, use gold water, do not add a magnetic code on the grinding head (the grinding head itself is 65g), and rub back and forth 10 times. Two test pieces are required for each gold water, and the outer cloth piece on the grinding head must be replaced before each test piece is measured. If the results of the two test pieces are inconsistent, a third test piece must be measured, and the two closest test pieces are taken as the final results. 3.10.3 Result judgment
Observe the friction center, and it is qualified if there is no gold removal and bottom exposure. 3.11 Determination of precipitation rate
3.11.1 Reagent
-Cyclohexanone, AR.
3.11.2 Instruments
Analytical balance, graduation value 0.1mg,
Constant temperature drying oven, maximum temperature not less than 200℃; centrifugal sedimentation machine, speed not less than 2500t/min flat weighing bottle, 5cm.
3.11.3 Determination steps
Take a piece of slow quantitative filter paper, fold it and put it in the weighing bottle, open the bottle mouth and dry it in a constant temperature drying oven at 105-110℃ for 1h, cover the bottle cap, move it to a dryer to cool for 40min and weigh it, repeat the operation until constant weight (W,). Then take the prepared gold water sample, shake it fully, so that the precipitate does not adhere to the bottom of the bottle, and then transfer it all to the filter paper with constant weight for filtration (when filtering, the liquid level should not exceed half the height of the filter paper, the same below), and wash it with a small amount of cyclohexanone - once or twice. The filtrate is collected in a clean beaker and transferred to the original filter paper for filtering again. The gold water bottle and beaker are cleaned with cyclohexanone, and the obtained washing liquid is transferred to the filter paper for filtering. Finally, the gold water on the filter paper is completely washed away with cyclohexanone until the washing liquid is colorless. The filter paper with precipitation is folded and placed in the original weighing bottle, and the bottle mouth is opened and dried in a constant temperature drying oven at 105-110℃ for 1h. Cover the bottle cap and transfer it to a dryer to cool for 40 min, take it out, weigh it, and repeat the operation until the constant weight (W). The gold water precipitation rate T(%) is calculated according to formula (7): T(%) = (W - W)/GX 100
Wt—the mass of the filter paper and weighing bottle before filtration, g; WL—the mass of the filter paper and weighing bottle after filtration + g, G—the net mass of the whole bottle of gold water, nom.
The deviation of parallel determination is not more than 0.04%.
3.12 Hiding power test
Only glass gold water is tested.
Under the gold layer thickness of the standard coating area (see 3.6), at a distance of 50cm, look directly at the light, and visually inspect the fired test piece. If there is no obvious light transmission phenomenon, it is qualified.6 Determination of coated area
Put more than 23gold water in a clean small glass bottle and insert a brush (the pen holder can be cut short for easy operation). After weighing the mass, take out the brush with gold water and draw a rectangular block roughly equal to 3cm×5cm on the porcelain or glass test piece. The coating thickness of the whole piece should be uniform. After drawing, put the pen back to the original bottle and weigh the mass again. The difference between the two masses is the amount of gold water consumed G. Use a ruler to measure the length and width of the coating gap (accurate to 0.1cm) and calculate the area S. The ratio of S to G is the coating area. If the batch value does not meet the specified value, it is necessary to re-coat the piece according to the method until it meets the requirements.
37 Determination of drying speed
Use a gold drawing pen to dip an appropriate amount of gold water sample, and draw 20 thick and thin parallel lines or cross lines with different thickness on the clean and dry porcelain piece according to the usual gold drawing thickness. After the test, record the time, place the test piece at room temperature of about 25℃ or in a constant temperature box, and gently touch the gold wire with your finger every 10 minutes. When the gold wire of medium thickness does not stick to your finger, record the time. The difference between the two times is the drying speed. 3.8 Color firing temperature test
Apply two test pieces of standard area according to the method in 3.6, and fire at the upper and lower limits of the color firing temperature respectively. Color firing method: Place one of the test pieces in the center of the muffle furnace, below the tip of the thermocouple, and use a refractory rack to support the test piece so that it is ? cm high from the bottom of the furnace. Close the furnace door, turn on the power to heat it. Before 400℃, the furnace door should leave a small gap to exhaust smoke. After 400℃, close the furnace door tightly and burn it to the lower limit temperature specified in this standard. Keep it for 15 minutes and then turn off the power. Cool it with the furnace door half open, and take out the test piece. Heat the other test piece to the upper limit temperature according to the same method, keep it at the upper limit temperature for 10 minutes, cool it, and take out the test piece.
Check the adhesion of the gold layer of the test pieces at each temperature, and check whether the test pieces burned to the upper limit temperature have discoloration. The test pieces with strong adhesion and no discoloration are qualified.
3.9 Gold burning test
Apply three porcelain or glass test pieces according to the method in 3.6, and place them in a muffle furnace to burn within the range of this standard. Observe the gold blocks made. The gold should be bright and free of contamination and other colors. When measured at a distance of 50mm, the three blocks are allowed to have only one circular spot with a diameter not greater than 0.3mm, except for spots (non-circular) caused by impurities brought in due to lax operation. Note: For new brushes that are glued, they should be filtered with water and cleaned of adhesives before use, and then dried. 3.10 Adhesion test
3.10.1 Instruments and materials
JMY gold abrasion tester:
50mm×50mm smooth glazed flat porcelain pieces: -50mm×50mmx3mm flat window glass pieces -Pure cotton cloth, pre-boil with water and rub to remove the glue. After drying, cut into 10 pieces of 32mm round shape, and store in a safe place. 281
3.10.2 Steps
QB/T 2382—1998
Apply gold water to two pieces of standard push area according to the method in 3.6, fire within the standard range, keep warm for 15 minutes, take out the test piece and place it in the room for about 4 hours, and then fix it on the gold abrasion tester sample table. Place five layers of cotton cloth on the grinding head and conduct a counting friction test. For porcelain and pond porcelain, use gold water, place a 500g magnetic code on the grinding head in advance, and rub back and forth 100 times: for glass and fine pottery, use gold water, do not add a magnetic code on the grinding head (the grinding head itself is 65g), and rub back and forth 10 times. Two test pieces are required for each gold water, and the outer cloth piece on the grinding head must be replaced before each test piece is measured. If the results of the two test pieces are inconsistent, a third test piece must be measured, and the two closest test pieces are taken as the final results. 3.10.3 Result judgment
Observe the friction center, and it is qualified if there is no gold removal and bottom exposure. 3.11 Determination of precipitation rate
3.11.1 Reagent
-Cyclohexanone, AR.
3.11.2 Instruments
Analytical balance, graduation value 0.1mg,
Constant temperature drying oven, maximum temperature not less than 200℃; centrifugal sedimentation machine, speed not less than 2500t/min flat weighing bottle, 5cm.
3.11.3 Determination steps
Take a piece of slow quantitative filter paper, fold it and put it in the weighing bottle, open the bottle mouth and dry it in a constant temperature drying oven at 105-110℃ for 1h, cover the bottle cap, move it to a dryer to cool for 40min and weigh it, repeat the operation until constant weight (W,). Then take the prepared gold water sample, shake it fully, so that the precipitate does not adhere to the bottom of the bottle, and then transfer it all to the filter paper with constant weight for filtration (when filtering, the liquid level should not exceed half the height of the filter paper, the same below), and wash it with a small amount of cyclohexanone - once or twice. The filtrate is collected in a clean beaker and transferred to the original filter paper for filtering again. The gold water bottle and beaker are cleaned with cyclohexanone, and the obtained washing liquid is transferred to the filter paper for filtering. Finally, the gold water on the filter paper is completely washed away with cyclohexanone until the washing liquid is colorless. The filter paper with precipitation is folded and placed in the original weighing bottle, and the bottle mouth is opened and dried in a constant temperature drying oven at 105-110℃ for 1h. Cover the bottle cap and transfer it to a dryer to cool for 40 min, take it out, weigh it, and repeat the operation until the constant weight (W). The gold water precipitation rate T(%) is calculated according to formula (7): T(%) = (W - W)/GX 100
Wt—the mass of the filter paper and weighing bottle before filtration, g; WL—the mass of the filter paper and weighing bottle after filtration + g, G—the net mass of the whole bottle of gold water, nom.
The deviation of parallel determination is not more than 0.04%.
3.12 Hiding power test
Only glass gold water is tested.
Under the gold layer thickness of the standard coating area (see 3.6), at a distance of 50cm, look directly at the light, and visually inspect the fired test piece. If there is no obvious light transmission phenomenon, it is qualified.3 Result judgment
Observe the friction center, if there is no gold removal and bottom exposure phenomenon, it is qualified. 3.11 Determination of precipitation rate
3.11.1 Reagents
-Cyclohexanone, AR.
3.11.2 Instruments
Analytical balance, graduation value 0.1mg,
Constant temperature drying oven, the highest temperature is not less than 200℃; centrifugal sedimentation machine, the speed is not less than 2500t/min flat weighing bottle, 5cm.
3.11.3 Determination steps
Take a piece of slow quantitative filter paper, fold it and put it in the weighing bottle, open the bottle mouth and dry it in a constant temperature drying oven at 105-110℃ for 1h, cover the bottle cap, move it to a dryer to cool for 40min and weigh it, repeat the operation until constant weight (W,). Then take the prepared gold water sample, shake it thoroughly to make the precipitate not adhere to the bottom of the bottle, and then transfer it all to the filter paper with constant weight for filtration (when filtering, the liquid level should not exceed half the height of the filter paper, the same below), and wash it with a small amount of cyclohexanone once or twice. The filtrate is used to receive the clean beaker and transferred to the original filter paper for filtration again. The gold water bottle and beaker are cleaned with cyclohexanone, and the obtained washing liquid is transferred to the filter paper for filtration. Finally, the gold water on the filter paper is washed with cyclohexanone until the washing liquid is colorless. Fold the filter paper with the precipitate and place it in the original weighing bottle, open the bottle mouth and dry it in a constant temperature drying oven at 105-110℃ for 1h. Cover the bottle cap and move it into the dryer to cool for 40 minutes, take it out, weigh it, and repeat the operation until the constant weight (W). The precipitation rate of gold water T(%) is calculated according to formula (7): T(%) = (W - W)/GX 100
Wt—the mass of filter paper and weighing bottle before filtration, g; WL—the mass of filter paper and weighing bottle after filtration + g, G—the net mass of the whole bottle of gold water, nom.
The deviation of parallel determination shall not exceed 0.04%.
3.12 Hiding power test
Only glass gold water is tested.
Under the gold layer thickness of the standard brushing area (see 3.6), at a distance of 50cm, look directly at the light, and visually inspect the fired test piece. If there is no obvious light transmission phenomenon, it is qualified.3 Result judgment
Observe the friction center, if there is no gold removal and bottom exposure phenomenon, it is qualified. 3.11 Determination of precipitation rate
3.11.1 Reagents
-Cyclohexanone, AR.
3.11.2 Instruments
Analytical balance, graduation value 0.1mg,
Constant temperature drying oven, the highest temperature is not less than 200℃; centrifugal sedimentation machine, the speed is not less than 2500t/min flat weighing bottle, 5cm.
3.11.3 Determination steps
Take a piece of slow quantitative filter paper, fold it and put it in the weighing bottle, open the bottle mouth and dry it in a constant temperature drying oven at 105-110℃ for 1h, cover the bottle cap, move it to a dryer to cool for 40min and weigh it, repeat the operation until constant weight (W,). Then take the prepared gold water sample, shake it thoroughly to make the precipitate not adhere to the bottom of the bottle, and then transfer it all to the filter paper with constant weight for filtration (when filtering, the liquid level should not exceed half the height of the filter paper, the same below), and wash it with a small amount of cyclohexanone once or twice. The filtrate is used to receive the clean beaker and transferred to the original filter paper for filtration again. The gold water bottle and beaker are cleaned with cyclohexanone, and the obtained washing liquid is transferred to the filter paper for filtration. Finally, the gold water on the filter paper is washed with cyclohexanone until the washing liquid is colorless. Fold the filter paper with the precipitate and place it in the original weighing bottle, open the bottle mouth and dry it in a constant temperature drying oven at 105-110℃ for 1h. Cover the bottle cap and move it into the dryer to cool for 40 minutes, take it out, weigh it, and repeat the operation until the constant weight (W). The precipitation rate of gold water T(%) is calculated according to formula (7): T(%) = (W - W)/GX 100
Wt—the mass of filter paper and weighing bottle before filtration, g; WL—the mass of filter paper and weighing bottle after filtration + g, G—the net mass of the whole bottle of gold water, nom.
The deviation of parallel determination shall not exceed 0.04%.
3.12 Hiding power test
Only glass gold water is tested.
Under the gold layer thickness of the standard brushing area (see 3.6), at a distance of 50cm, look directly at the light, and visually inspect the fired test piece. If there is no obvious light transmission phenomenon, it is qualified.
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