GB/T 15080.9-1994 Chemical analysis methods for antimony concentrates - Determination of gold content
Some standard content:
National Standard of the People's Republic of China
Chemical Analysis Method of Antimony Concentrates
Antimnny cnncenirates--Deterntinution of gold cnntent
1 Subject Content and Applicable Scopebzxz.net
This standard specifies the determination method of gold content in antimony concentrates. This standard is applicable to the determination of gold content in antimony concentrates. Determination range: 1g/t~~40/t. 2 Reference Standards
GB1.4 Standardization Guidelines for Standardization Chemical Analysis Methods Standard Preparation Provisions GB1457 General Principles and General Provisions for Chemical Analysis Methods of Metallurgical Products 3 Method Summary
CB/T15080.9-94
While melting the sample with an appropriate amount of flux, lead is used to capture gold and separate it from impurities; gold, silver and base metals such as lead are separated by ash blowing; gold and silver are separated by the property that gold is insoluble in nitric acid: and the weight method is used to determine gold. 4 Reagents and materials
4.1 Sodium carbonate, 1.1% industrial pure, anhydrous, powdered. 4.2 Zirconia, industrial pure, containing less than 0.05 gt, 4.3 Silicon dioxide, 1.1% industrial pure (SiO2>95%), powdered. 4.4 Borax, industrial pure, powdered.
4.5 Potassium nitrate, industrial pure, powdered,
4.6 Starch, 1.1% industrial pure.
4.7 Nitride, industrial pure,
4.8 Acetic acid (1+3), not ionized.
4.9 Nitric acid (1+7), not containing arsenic ions,
4.10 Silver nitrate solution (160 g/1.1), stored in a brown dropper bottle. 4.11 When testing gold, use a shaped ball made of refractory clay, with an outer diameter of 85~95 mm at the top and 50~60 mm at the bottom. The height is 110 mm and the volume is 100-320 ml. 4.12 Magnesium sand ash: Mix 8.3 kg of magnesium sand containing more than 83% magnesium oxide and a particle size of 0.15-0.25 mm with 1.5 kg of 425 silicate mud, then mix with 1 kg of water, and use a ash machine to press it into an inner diameter of about 35 mm and a depth of about 17 mm. Use it after natural drying for one month. 5 Equipment and instruments 5.1 Box-type electric furnace. The maximum overflow temperature is 1 350C. Approved by the State Administration of Technical Supervision on May 11, 1994
Implemented on December 1, 1994
5.2 Box-type electric furnace, maximum temperature 950℃, 5.3 Balance, maximum sensitivity 0.01g.
5.4 Day, maximum sensitivity 0.01 mg.
5.5 Day, maximum sensitivity 0.001mg.
6 Sample
6.1 The sample particle size should be less than 0.074 mm. CB/T 15080.9-94
6.2 The sample should be dried at 10~105℃ for 1.5 h, placed in a desiccator, and cooled to air humidity. 7 Analysis steps
7.1 Sample
Weigh 10:00~20.008 sample, accurate to 0.01g. Three measurements are made independently and the average value is taken. 7.2 Blank test
A blank test is performed with the sample D in Table 1. If the average value of the three results of the gold content in lead oxide is less than 0.05/t, the blank value is not included in the calculation. If it is greater than 0.05g/t, the lead oxide needs to be replaced. 7.3 Ingredients
7.3.1 Silica: Control between 0.5~1.5. When the antimony and sulfur content is high, 0.5~1.0 is selected; when the potassium, sulfur content is low and the silicon content is low, 1.0~-1.5 is selected.
Depending on the gold content and impurity content in the sample, select from the three ingredients A, B, and C in Table 1. Table 1
Test material +
Sodium carbonate
7.3.3 Added amount of potassium carbonate or starch:
7.3.3.1 Calculation method:
Calculate the total reducing power of the test material according to formula (1):
Wu Zhong, F, total reducing power of the test material
S percentage of sulfur in the test material, %
m——mass of the test material g
Oxide g
Silicon dioxide
11. 0--13. 0
9. ~-12. 0
F,=mu×s×23
281Sulfur can be reduced to an empirical value of about 23% by weight. 7.3.3.2 Determination method:
The total reducing power in the test material is determined by the reducing power method. Sand g
Potassium nitrate, g
Starch +
Prepare the ingredients A in Table 1 as potassium nitrate and starch, and operate according to 7.4.1 and 7.4.2. Weigh the mass of the obtained lead puff, and calculate the reducing power of the sample using formula (2).
Where: F,——reducing power of 1g sample; mi
Mass of lead puff, g:
moMass of sample, g.
Total reducing power of the sample:
GB/T 15080.9-94
F. = m,F,
7.3.3.3 Calculate the amount of potassium nitrate or starch added based on the total reducing power: When F,>30, add potassium nitrate during batching, and its amount is: F,-30
When F,<≤30, add starch during batching, and its amount is 30-F.
7.4 Determination
(3)
(4)
7.4.1 Put the sample and flux into the assay crucible (4.11) according to the batching of 7.3.2, and add 0.1~0.15 mL of silver nitrate solution (4.10).
7.4.2 Melt. Heat the box-type electric furnace (5.1) to 850-1000℃, put the assay crucible with the sample and flux into the furnace, raise the furnace temperature to 1180℃ within 50-60 minutes, take out the assay crucible, rotate it steadily for 2-3 times, gently drum it twice, and carefully pour the molten material into a conical iron mold that has also been dried and coated with engine oil. After cooling, remove the slag on the surface of the lead buckle and hammer it into a cube. The weight of the lead buckle should be controlled between 25 and 40°C.
7.4.3 Ash blowing. Put the ash (4.12) into the electric furnace (5.2), heat it to 930℃, and keep it for 15 minutes. Put the lead buckle into the ash, close the furnace door, open the furnace door slightly after the molten lead is stripped, keep 900℃ (±20℃), and stop the ash blowing after the flash appears, and remove the ash from the furnace.
7.4.4 Gold separation: Take out the gold and silver particles from the ash and blood, clean the ash and blood, hammer them into thin slices on an anvil, put them in 30mL of porcelain crucible, add 20mL of nitric acid (4.9) at about 90℃, separate the gold in a boiling water bath, after the silver reaction stops, remove the crucible, wash it with hot water once, then add 20mL of nitric acid (4.8) at about 90℃, separate the gold at a temperature slightly higher than the first gold separation for 20min, pour out the solution, wash the gold particles and the crucible with hot water for 2~3 minutes, dry them, burn them at 600℃ for 5min, cool them, and weigh the gold particles on a balance (5.4 or 5.5). 8 Expression of analysis results
Calculate the gold content according to formula (5):
Auig/t)
Where: m—mass of gold particles, mg,
mass of sample,.
m×1000
（5）
The analysis results shall be expressed to two decimal places.
9Tolerance
GB/1 15080-9--94
The difference in analysis results between laboratories shall not be greater than the allowable difference listed in Table 2. Table 2
Gold content
.2. 00
2-2. 00~3. 00
3. 00~ 5. 00
>5. 00~7. 00
7.00-~10. 00
210. 00~ 15. 00
>15, 00~ 20, 00
>20. 00 ~ 30. 00
>30.00~40.00
Additional remarks:
This standard was proposed by China Nonferrous Metals Industry Corporation. This standard was technically classified by Beijing Research Institute of Mining and Metallurgy. This standard was drafted by Xikuangshan Mining Bureau and Hunan Nonferrous Metals Research Institute. This standard was drafted by Hunan Nonferrous Metals Research Institute. The main drafter of this standard is Liu Quanquan.
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