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GB/T 10046-2018 English PDF (GBT10046-2018)

GB/T 10046-2018 English PDF (GBT10046-2018)

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GB/T 10046-2018: Silver brazing filler metals

This Standard specifies the requirements such as model, technical requirements, test methods, inspection rules, packaging, marking, quality certification of silver brazing filler metals. This Standard applies to silver brazing filler metals used in brazing methods.
GB/T 10046-2018
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 25.160.50
J 33
Replacing GB/T 10046-2008
Silver brazing filler metals
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(ISO 17672:2016, Brazing - Filler metals, MOD)
ISSUED ON: MAY 14, 2018
IMPLEMENTED ON: DECEMBER 01, 2018
Issued by: State Administration for Market Regulation;
Standardization Administration of the PRC.
Table of Contents
Foreword ... 4
1 Scope ... 7
2 Normative references ... 7
3 Model ... 8
3.1 Method of model preparation ... 8
3.2 Model example ... 8
4 Technical requirements ... 8
4.1 Product form ... 8
4.2 Chemical composition ... 9
4.3 Dimensions and tolerances ... 13
4.4 Supply status ... 15
5 Test methods ... 15
5.1 Chemical composition analysis of brazing filler metals ... 15
5.2 Mechanical property test of brazed and soldered joint ... 15
5.3 Wettability test of brazing filler metals ... 15
6 Inspection rules ... 16
6.1 Heat number division ... 16
6.2 Sampling method ... 16
6.3 Acceptance ... 16
6.4 Reinspection ... 16
7 Packaging, marking, quality certification ... 17
7.1 Packaging ... 17
7.2 Marking ... 17
7.3 Quality certification ... 17
Annex A (Informative) Structural changes of this Standard compared with ISO 17672:2016 ... 18
Annex B (Normative) Determination of silver content ... 19
Annex C (Normative) Determination of copper content - Electrolysis-
spectrophotometry ... 24
Annex D (Normative) Determination of zinc and cadmium content - EDTA
titration method ... 29
Annex E (Normative) Determination of nickel content ... 35
Annex F (Normative) Determination of tin content - Potassium iodate titration method ... 43
Annex G (Normative) Determination of lithium content - Atomic absorption spectrometry ... 48
Annex H (Normative) Determination of indium content ... 52
Annex I (Normative) Determination of aluminum content - Sodium fluoride replacement -EDTA titration method ... 59
Annex J (Normative) Determination of manganese content ... 63
Annex K (Normative) Inductively coupled plasma atomic emission spectrometry ... 69
Annex L (Informative) Model comparison of brazing filler metals ... 79
Silver brazing filler metals
1 Scope
This Standard specifies the requirements such as model, technical
requirements, test methods, inspection rules, packaging, marking, quality certification of silver brazing filler metals.
This Standard applies to silver brazing filler metals used in brazing methods. 2 Normative references
The following documents are indispensable for the application of this document. For the dated references, only the editions with the dates indicated are applicable to this document. For the undated references, the latest edition (including all the amendments) are applicable to this document.
GB/T 6682 Water for analytical laboratory use - Specification and test
methods (GB/T 6682-2008, ISO 3696:1987, MOD)
GB/T 8170 Rules of rounding off for numerical values and expression and judgement of limiting values
GB/T 11363 Test method of the strength for brazed and soldered joint (GB/T 11363-2008, ISO 5187:1985, NEQ)
GB/T 11364 Test method of wettability for brazing filler metals (GB/T 11364- 2008, ISO 5179:1983, NEQ)
GB/T 12806 Laboratory glassware - One-mark volumetric flasks (GB/T
12806-2011, ISO 1042:1998, NEQ)
GB/T 12808 Laboratory glassware - One mark pipettes
GB/T 12809 Laboratory glassware - Principles of design and construction of volumetric glassware (GB/T 12809-2015, ISO 384:1978, NEQ)
GB/T 12810 Laboratory glassware - Volumetric glassware - Methods for use and testing of capacity (GB/T 12810-1991, ISO 4787:1984, IDT)
6 Inspection rules
Finished brazing filler metals are inspected by the manufacturer's quality inspection department according to the heat number.
6.1 Heat number division
The definition of heat number of brazing filler metals depends on the method of smelting and refining, as follows:
- In the metal smelting process, slag-metal or gas-metal reactions occur. The heat number refers to the material obtained from the same furnace smelting. - In the metal smelting process, no obvious chemical reactions occur (such as induction melting or vacuum melting in a controlled atmosphere). The heat number refers to a group of materials obtained by continuous smelting under the same conditions in a smelting furnace, using one lot of metals and alloy elements with controlled burden. And the chemical composition of each furnace of smelting material is in line with the purchaser or brazing filler metal manufacturer's specified range.
6.2 Sampling method
During the inspection of each furnace of brazing filler metals, according to the required quantity, representative samples shall be taken from at least three locations. The sampling method and sampling location shall be recorded. 6.3 Acceptance
The manufacturer of brazing filler metals shall, in writing, provide the main performance parameters such as chemical composition, dimensions,
appearance of brazing filler metals; declare that "when tested in accordance with this Standard, the brazing filler metals provided meet the requirements of this Standard".
6.4 Reinspection
When any one of the inspections fails, this item shall be double reinspected. For the chemical composition analysis of brazing filler metals, only those elements that do not meet the requirements are reinspected. The results of the doubled reinspection shall meet the requirements of this item.
If the reinspection result is still unqualified, brazing filler metals in this furnace cannot be delivered as finished products, which meet this Standard.
Annex B
(Normative)
Determination of silver content
B.1 Silver chloride gravimetric method
B.1.1 Scope
This method is suitable for the determination of silver content in silver brazing filler metals. Determination range (mass fraction): 25.0%~99.95%.
B.1.2 Method summary
USE nitric acid to decompose the test portion. If there is precipitation, after filtration, add hydrochloric acid to form silver chloride precipitation; USE a glass crucible to separate it; and, weigh its mass after drying (the filtrate may be used to determine the copper content).
B.1.3 Reagents
B.1.3.1 Nitric acid (1+1).
B.1.3.2 Nitric acid (1+100).
B.1.3.3 Hydrochloric acid (1+9).
B.1.4 Analytical procedures
B.1.4.1 Test portion
WEIGH 1.0 g of sample, accurate to 1 mg.
B.1.4.2 Determination
B.1.4.2.1 PLACE the weighed test portion (B.1.4.1) in a 300 mL tall beaker; ADD 10 mL of nitric acid (B.1.3.1) and cover with a watch glass; slowly heat to decompose; BOIL to allow nitrogen oxides to escape. USE water to rinse the inner wall of the beaker; ADD warm water to 50 mL. At this time, if there is precipitation, it shall let it stand for 1 h in a place where the temperature is slightly higher; then use slow-speed filter paper to filter it. USE hot nitric acid (B.1.3.2) to wash the precipitation.
B.1.4.2.2 ADD water to 150 mL; while stirring, add hydrochloric acid (B.1.3.3) solution after calibration, in moles per liter (mol/L);
V0 - The value of the volume of ammonium thiocyanate standard titration solution consumed for calibration, in milliliters (mL);
107.868 - The value of the molar mass of silver, in grams per mole (g/mol). Calibrate three parts in parallel. The range of the volume of the ammonium thiocyanate standard titration solution consumed shall not exceed 0.10 mL. TAKE the average. Otherwise, re-calibrate.
B.2.4 Analytical procedures
B.2.4.1 Test portion
WEIGH 0.50 g of sample, accurate to 1 mg.
B.2.4.2 Determination
B.2.4.2.1 PLACE the weighed test portion (B.2.4.1) in a 300 mL conical beaker; ADD 15 mL of nitric acid (B.2.3.1) and cover with a watch glass; slowly heat to decompose; BOIL to allow nitrogen oxides to escape. After cooling, use water to rinse the inner wall of the beaker; then add water to dilute to 150 mL. B.2.4.2.2 ADD 3 mL of ferric ammonium sulfate solution (B.2.3.2) as an
indicator; while shaking, use ammonium thiocyanate standard titration solution (B.2.3.3) to titrate, until the solution just appears reddish-brown, which is the end point.
B.2.5 Expression of analysis results
The silver content is expressed in (Ag). The value is expressed in %, calculated according to formula (B.3):
Where:
c - The actual concentration value of ammonium thiocyanate standard titration solution after calibration, in moles per liter (mol/L);
V - The value of the volume of ammonium thiocyanate standard titration solution consumed in the titration, in milliliters (mL);
m0 - The value of the mass of test portion, in grams (g);
107.868 - The value of the molar mass of silver, in grams per mole (g/mol). Annex C
(Normative)
Determination of copper content - Electrolysis-spectrophotometry
C.1 Scope
This annex applies to the determination of copper content in silver brazing filler metals. Determination range (mass fraction): 14.00%~60.00%.
C.2 Method summary
USE nitric acid to decompose the test portion; ADD hydrochloric acid for precipitation to separate silver; USE sulfuric acid to smoke away hydrochloric acid; after cooling, add water and nitric acid for low-current electrolysis. After the electrolysis is terminated, the platinum cathode is washed using water and absolute ethanol, dried, cooled, and then weighed. USE spectrophotometry to measure the copper content remaining in the solution after electrolysis and correct it to obtain the copper content.
C.3 Reagents
C.3.1 Absolute ethanol.
C.3.2 Nitric acid (1+1).
C.3.3 Nitric acid (1+100).
C.3.4 Hydrochloric acid (1+9).
C.3.5 Sulfuric acid (1+1).
C.3.6 Aqueous ammonia (1+1).
C.3.7 Ammonium citrate solution (500 g/L).
C.3.8 Dicyclohexanone oxalyl dihydrazone (BCO) solution (1 g/L): WEIGH 0.5 g of BCO in a 300 mL beaker; ADD 50 mL of ethanol, 200 mL of warm water to dissolve; TRANSFER to a 500 mL volumetric flask; USE water to dilute to the mark and mix well.
C.3.9 Copper standard stock solution: WEIGH 0.1000 g of pure copper into a 150 mL beaker; ADD 10 mL of nitric acid (C.3.2) and cover with a watch glass; MAKE it completely decomposed at low temperature; BOIL to remove nitrogen replace it with another tall beaker containing 180 mL of water; continue electrolysis for 15 min.
C.5.2.6 Immediately take out the platinum electrode and immerse it in another 250 mL beaker filled with water; MOVE it up and down 3 times. TURN off the power and remove the electrode; PUT it in a beaker containing absolute ethanol (C.3.1); TAKE it out and place it in a 105 ??C electrothermal constant-
temperature drying oven for drying for 3 min~5 min; then take it out and place it in a desiccator to cool to room temperature.
C.5.2.7 WEIGH the platinum electrode after electrolytic deposition of copper, accurate to 0.0001 g.
C.5.2.8 According to the following method, determine the amount of residual copper in the solution after electrolysis.
C.5.2.8.1 Blank test: TAKE 10 mL of sulfuric acid (C.3.5), 5 mL of nitric acid (C.3.2) in a 500 mL volumetric flask; do a blank test with the test portion. C.5.2.8.2 COMBINE the electrolyte after electrolysis and a glass of water obtained from electrolysis for 15 min into a 500 mL volumetric flask; USE water to dilute to the mark and mix well.
C.5.2.8.3 PIPETTE 10.00 mL~20.00 mL of solution into a 50 mL volumetric flask; ADD 2 mL of ammonium citrate solution (C.3.7); USE water to dilute to about 25 mL; ADD 2~3 drops of neutral red ethanol solution (C.3.11). USE aqueous ammonia solution (C.3.6) to neutralize, until the red color fades and add 1.0 mL in excess. ADD 8.0 mL of BCO solution (C.3.8); USE water to dilute to the mark and mix well; and let stand for 20 min.
C.5.2.8.4 USE a 2 cm cuvette; USE the blank test as a reference. At a
wavelength of 600 nm, measure the absorbance; FIND out the corresponding amount of copper from the working curve.
C.5.2.8.5 Drawing of working curve
PIPETTE 6 parts of 20.00 mL of blank solution (C.5.2.8.1); PLACE them in a set of 50 mL volumetric flasks. ADD 0 mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL, 5.00 mL of copper standard solution respectively. Then proceed according to C.5.2.8.3 and C.5.2.8.4. USE copper content as the abscissa and absorbance as the ordinate; DRAW the working curve.
C.6 Expression of analysis results
The copper content is expressed in ??(Cu). The value is expressed in %,
calculated according to formula (C.1):
Annex D
(Normative)
Determination of zinc and cadmium content - EDTA titration method
D.1 Scope
This annex applies to the determination of zinc content in silver brazing filler metals. Determination range (mass fraction): 4.00%~45.00%.
This annex applies to the determination of cadmium content in silver brazing filler metals. Determination range (mass fraction): 10.00%~30.00%.
D.2 Method summary
USE nitric acid to decompose the test portion. The tin is removed by
metastannic acid precipitation and filtration. USE silver chloride precipitation method to separate silver, electrolysis method to separate copper. Adjust the solution after separation of silver and copper to ammoniac. Indium and nickel are separated by filtration in the form of hydroxide precipitation and
dimethylglyoxime nickel precipitation, respectively. Adjust the pH value within the range of 5.5~6.5; USE thiourea to mask the remaining copper and silver; USE EDTA standard titration solution to titrate the total amount of zinc and cadmium. ADD excess potassium iodide to the test solution to release the EDTA in Cd-EDTA; then use zinc standard solution to back-titrate the released EDTA, to indirectly measure the cadmium content. Zinc is calculated by subtraction method.
D.3 Reagents
D.3.1 Potassium iodide, analytically pure.
D.3.2 Ammonium persulfate, analytically pure.
D.3.3 Nitric acid (1+1).
D.3.4 Nitric acid (3+100).
D.3.5 Hydrochloric acid (1+1).
D.3.6 Hydrochloric acid (1+99).
D.3.7 Sulfuric acid (1+1).
TAKE 3 parts for calibration. The range of the volume of the consumed EDTA standard titration solution does not exceed 0.10 mL. TAKE the average.
Otherwise, re-calibrate.
D.3.15 Xylenol orange solution (2.5 g/L).
D.4 Apparatus
D.4.1 Electrolysis device equipped with automatic stirring device, precision ammeter and voltmeter.
D.4.2 Platinum cathode: USE a platinum wire with a diameter of 0.2 mm to weave into a mesh with a mesh size of about 36 ??m per square centimeter, to make a mesh cylinder (see Figure C.1 in Annex C).
D.4.3 Platinum anode: Spiral (see Figure C.2 in Annex C).
D.5 Analytical procedures
D.5.1 Test portion
WEIGH 0.40 g of sample, accurate to 1 mg.
D.5.2 Determination
D.5.2.1 PLACE the test portion (D.5.1) in a 250 mL beaker.
D.5.2.2 ADD 5 mL of nitric acid (D.3.3); COVER with a watch glass; slowly heat to decompose the test portion; REMOVE nitrogen oxides, remove and cool. D.5.2.3 USE water to rinse the watch glass and beaker wall; HEAT and
evaporate at a low temperature to make the solution volume about 5 mL. Take off and wash the watch glass and beaker wall. Adjust the volume to about 50 mL; HEAT it at a low temperature for 10 min~20 min; REMOVE it to cool.
D.5.2.4 USE medium-speed double-layer quantitative filter paper to filter by decanting method. USE hot nitric acid (D.3.4) to wash the precipitate in the beaker 3 times; then move the precipitate into the funnel; continue to use nitric acid (D.3.4) to wash the precipitate in the beaker and the funnel 8~10 times. DISCARD the precipitate and adjust the volume of the filtrate to about 120 mL. D.5.2.5 While stirring, add 2 mL of hydrochloric acid (D.3.5); COVER with a watch glass; HEAT at low temperature to make the solution clear and remove it.
D.5.2.6 USE quantitative filter paper to filter by decanting. USE hot hydrochloric acid (D.3.6) to wash the precipitate in the beaker 3 times; then transfer the precipitate into the funnel; continue to use hot hydrochloric acid (D.3.6) to wash the precipitate in the beaker and the funnel 8~10 times. DISCARD the
precipitate.
D.5.2.7 ADD 2 mL of sulfuric acid (D.3.7) to the filtrate; evaporate to smoke, cool; ADD water and 5 mL of nitric acid (D.3.3) to dissolve the salts; adjust the volume of the solution to about 150 mL. INSERT the platinum electrode pre- installed on the electrolysis device into the solution; USE two semicircular watch glasses to cover the beaker; under stirring, electrolyze with 2 A~2.5 A current, until the blue color disappears; rinse the watch glasses and the beaker wall; continue electrolysis for 2 h~3 h. Without disconnecting the current, move the electrode up and leave the liquid surface. USE water to rinse the electrode; then disconnect the power supply. HEAT and evaporate to adjust the volume of the electrolyte to about 120 mL.
D.5.2.8 ADD aqueous ammonia (D.3.8) to the electrolyte, until a strong
ammonia smell appears in the test solution; and then add 5 mL in excess. ADD 1 g of ammonium persulfate (D.3.2) and boil for 1 min. COOL to room
temperature; TRANSFER the solution into a 200 mL volumetric flask.
D.5.2.9 While shaking, add dimethylglyoxime ethanol solution (D.3.11) (add 7 mL of dimethylglyoxime ethanol solution (D.3.11) per 10 mg of nickel); COOL to room temperature; USE water to dilute to the mark and mix well; and dry filter. D.5.2.10 Accurately pipette 50.00 mL of filtrate into a 300 mL conical flask; ADD nitric acid (D.3.3) until the solution is acidic (can be tested with pH test paper); and then add 5 mL in excess. ADD 2 mL of thiourea solution (D.3.9), 40 mL of hexamethylenetetramine solution (D.3.10); then add 5 drops of xylenol orange indicator (D.3.15); USE EDTA standard titration solution (D.3.14) to titrate, until the solution turns from purple-red to yellow. RECORD the volume V1 of the EDTA standard titration solution. This is the volume of the EDTA standard titration solution consumed by zinc and cadmium.
D.5.2.11 ADD about 30 g of potassium iodide (D.3.1) to the test solution and shake well; HEAT and boil for 3 min until the test solution is clear, remove and cool. USE zinc standard solution (D.3.12) to titrate, until the solution becomes stable rose red. RECORD the volume V2 of the zinc standard solution (D.3.12) consumed. This is the volume of zinc standard solution consumed by EDTA released from Cd-EDTA.
Note 1: If there is no tin in the test portion, D.5.2.3~D.5.2.4 can be omitted. Note 2: If there is no nickel in the test portion, then D.5.2.8~D.5.2.9 and "ADD nitric acid (D.3.3) until the solution is acidic; and then add 5 mL in excess" in D.5.2.10 can be omitted.
Note 3: If there is no manganese in the test portion, then "ADD 1 g of ammonium persulfate (D.3.2) and boil for 1 min" in D.5.2.8 can be omitted.
Note 4: If the test portion contains only zinc, V1 is the volume of the EDTA standard solution consumed by zinc alone; the next step does not need to be performed.
D.6 Expression of analysis results
The zinc content is expressed in ??(Zn). The value is expressed in %, calculated according to formula (D.2):
Where:
c - The actual concentration value of the EDTA standard titration solution after calibration, in moles per liter (mol/L);
?? - The value of the concentration of zinc standard solution, in milligrams per milliliter (mg/mL);
V1 - The ...

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