This standard specifies the sampling and preparation methods of ferroalloy product samples for chemical analysis and the relevant accuracy requirements. This standard is applicable to the retest and arbitration of ferroalloy products. GB/T 4010-1994 Sampling and preparation of samples for chemical analysis of ferroalloys GB/T4010-1994 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Ferroalloys-sampling and preparation ofsamples for chemical analysisGB/T 4010—94
Replaces GB401083
GR 4332—84
This standard refers to and adopts the international standard ISO4552:1987 "Ferroalloys-Sampling and preparation of samples for chemical analysis". 1 Subject content and scope of application
This standard specifies the sampling and preparation methods of ferroalloy product samples for chemical analysis and the relevant accuracy requirements. This standard is applicable to the re-inspection and arbitration of ferroalloy products. 2 Referenced standards
GB/T13247 Sampling and detection methods for particle size of ferroalloy products 3 Sampling tools
3.1 Sampling shovel
The sampling shovel is shown in Figure 1. The dimensions of the sampling shovel are shown in Table 1. Figure 1
Maximum rated particle size, mm
Dimensions. mm
Note: When the rated maximum particle size is greater than 150mm, the portion sample shall be picked up manually or taken horizontally. Approved by the State Bureau of Technical Supervision on June 13, 1994 Material thickness
Implementation on January 1, 1995
3.2 Joint sample drill
Sampling drill See Figure 2:
Material specification: Seamless pipe
GB/T4010-94
Outer jacket; outer diameter 35 mm, wall thickness 2 mmi
Inner inspection: outer diameter 30 mm, wall friction 2 mm
Sampling comfort Used for sampling of ferroalloy product packages with a maximum particle size of no more than 4 mm, the effective length of the sampling nail shall be greater than 80% of the diagonal of the package.
Delivery (batch) products
4 Composition and reduction of large samples
4.1 Composition of individual samples
4.1.1 Direct composition of large samples.
4.1.2 First form sub-samples, then form individual samples.
4.2 Reduction of large samples
4.2.1 Samples with a particle size less than 10 mm will be reduced and divided into increments
Delivery (batch) products
4.2.2 The facilities for sample reduction should be thoroughly cleaned. A certain amount of the same iron silo should be passed through them once or more. 4.2.3 Before reduction, the sample components should be fully mixed for no less than 3 times. 4.2.4 Reduction method
4.2.4.1 Cone quartering method.
4.2.4.2 Grid reduction method.
4.2.4.3 Divider method,
4.2.4.4 Grid divider method.
4.2.5 Dividing procedure
4.2.5.1 Cone quartering method Dividing procedure,
GB/T 4010—94
Place the sample to be divided on a clean steel plate: stack it into a cone, a
b. Change the position and use the shovel grid to stack the samples in turn at the points of another circle, and try to make the large sample fall evenly at the bottom of the chain. Use this method until the original cone sample is completely transferred. Then repeat this operation once. c. Use a shovel or plate to press the third cone sample vertically from the top of the circle to flatten the sample. When flattening the sample, make the center of the shovel or plate coincide with the center point of the cone sample.
. Divide the flattened reading stand-shaped sample into four equal parts using two perpendicular lines at its center. Use the two diagonal parts as the weaving samples and discard the other two. Follow steps a to d above until the required number is reached. e.
4.2.5.2 Grid subdivision procedure:
4.2.5.2.1 The size of the subdivision spade shall be selected according to the particle size of the corresponding sample that is fully passed in Table 2. Table 2
Particle size of the sample that is fully passed, mm
Thickness of the spread sample, mm
25--35
Note: The size specified in Table 2 is shown in Figure 1
Cut off the front part of the spade in Figure 1 to make a flat spade for subdivision. 4.2.5.2.2 Subdivision steps
Size of the subdivision spade, mm
Material thickness
Leave the sample on the sliding surface (such as a steel plate) and spread it into a flat rectangle with a thickness specified in Table 2. b. Spread this rectangle The sample is equally divided into no less than 20 grids. According to the particle size through which all the samples pass, select the corresponding reduction shovel in Table 2. b/e
d Take out a full shovel of sample from each equally divided grid, and collect the taken samples as the reduction sample. When sampling, insert the shovel baffle vertically into the sample, and insert the shovel to the bottom of the sample, so that it is easy to remove the sample. e. When the weight of the taken reduction sample is less than the required test sample, either use a large reduction shovel or increase the number of sampling. 4.2.5.3 The binary divider method and the grid divider method shall be operated according to the equipment instruction manual. 5 Sampling and sample preparation of easily broken iron and gold
5.1 Comprehensive accuracy of the supplied chemical composition
When the confidence level of the supplied chemical composition is 95%, its comprehensive accuracy is shown in Table 3 And Table 4. Delivery batch
Delivery quantity
52 pieces
(Easy to break)
GB/T 4010—94
Comprehensive accuracy%
FeCtsi
FeMnSi
Comprehensive precisionBapm%
The minimum sample size corresponds to the rated maximum particle size of the batch of goods, which meets the requirements of Table 5. 0.56
Rated maximum
Particle size.TnTL
(Easy to break)
5.3 Number of samples and sampling accuracy
FeCrSi
GB/T 4010—94wwW.bzxz.Net
FeMnSi
The minimum number of samples and sampling accuracy shall comply with the requirements of Table 6 and Table 7 Table 6
Delivery batch
5 0100
(Easy to break)
Mixing accuracy%
FeCrsi
FrMnsi
Delivery batch
5.4 Sampling method
5.4.1 Bulk sampling
5.4.1.1 Manual sampling
GB/T 401094
Accuracy B%
In a batch of goods, the manual picking or smashing of the portion samples or the use of sampling shovels to take the portion samples shall be determined according to the particle size composition of the ferroalloy. The manual picking or taking of the portion samples may be carried out by random sampling or systematic sampling. The number of portion samples shall comply with the provisions of Table 6 and Table 7. The portion sample quantity shall be roughly the same and meet the requirements of Table 5. When using a sampling shovel to take the portion samples, first determine the sampling shovel according to the particle size composition of the ferroalloy and the batch size. Secondly, the random sampling method or systematic sampling method shall be used to take the portion samples. The number of portion samples shall comply with the provisions of Table 6 and Table 7. The portion sample quantity shall roughly meet the requirements of Table 5.
5.4.1.2 Mechanical sampling
When mechanical sampling is carried out, random sampling or systematic sampling may be used. The number of portion samples shall comply with the provisions of Table 6 and Table 7. The portion sample quantity shall roughly meet the requirements of Table 5.
5.4.2 Sampling of packages
Sampling of packages usually adopts a two-step sampling method, and random sampling or systematic sampling can be used in the sampling process. When the number of incremental samples specified in Tables 6 and 7 is less than the number of packages in the supply batch, at least the same number of incremental samples should be selected, and "incremental samples" should be taken from each package. When the number of incremental samples specified in Tables 6 and 7 is greater than the number of packages in the supply batch, 2 or more incremental samples can be selected from each package. The amount of incremental samples should be roughly the same and meet the requirements of Table 5.
5.4.3 When the rated maximum particle size is greater than 150mm, incremental samples can be picked up or smashed manually in the selected package; when the rated maximum particle size is not greater than 150mm, incremental samples can be taken from the selected package with a sampling shovel that meets the requirements of Table 1 (incremental samples can also be picked up manually); when the rated maximum particle size is not greater than 4 1n1, you can use the sampling needle that complies with 3.2 to take a portion sample in the selected package. 5.4.4 When taking samples with a sample rod, you should first close the mouth of the sample rod and insert it obliquely into the opened package. The insertion depth should be greater than 80% of the diagonal of the package. Turn the inner meter, open the slot to allow the powder to enter the sampling rod smoothly, then close the slot, take out the sampling rod, and take the sample in the rod as a portion sample. The weight of each portion sample taken is roughly the same, and the number and quantity of portions meet the relevant requirements of Tables 5 to 7. 5.5 Sample preparation
5.5.1 Accuracy of sample preparation When the confidence of the supplied chemical composition is 95%, the accuracy of sample preparation is shown in Table 8. Product Properties Light Element Preparation Mixing Han (easy to break) FetrSi GB/T 4010—94 HeMnSi GFeMin .150. 301 ±- 40 5.5.2 After the sample is broken, it is required to be sieved completely. According to the maximum particle size of the sample, the minimum sample amount left after the reduction is determined, see Table 9. Table 9 Maximum viscosity of the sample, mm1 Minimum weight of the sample after reduction, kg 5.5.3 The weight of the test sample for chemical analysis should not be less than 50 g. The maximum particle size of the test sample should not be greater than 0.16 mm. Note: The particle size of the analysis sample shall be prepared in accordance with the requirements of the corresponding analysis method: Appendix: FeSi test specimen (example)
Delivery batch 501
Rated maximum particle size is 100mm
Sample 120 kg
8kg×15
Crushed to -1Gmm
Sample weight after reduction 15 kg
Crushed to -2.8 mm
Sample weight after reduction 1.9 kg
Resolved to -1.0 mm
Sample weight after reduction 400 g
to -0.16 mm
Four test samples, each weighing 50 g
Reduction three times
Reduction once
Using the method of incremental sampling
6 Sampling and sample preparation for non-breakable ferroalloys
6.1 Comprehensive accuracy of chemical composition of supply
GB/T 4010—94
When the confidence level of chemical composition of supply is 95%, its comprehensive accuracy is shown in Table 10. Table 10
FeCr (non-breakable)
Delivery batch
6.2 Sample quantity
Comprehensive accuracy
Delivery batch
For non-breakable ferroalloys, the sample quantity drilled from each sample block should not be less than 20g. 6.3 Number of samples and sampling accuracy
For non-breakable ferroalloys, the minimum number of blocks to be sampled and the sampling accuracy are shown in Table 11. Table 11 FeCt (not easy to break) Delivery quantity Sampling accuracy Bey Delivery batch Comprehensive accuracy Bamn % Sampling accuracy Delivery batch FeCt (not easy to break) GB/T 4010—94
Continued Table 11
Accuracy of sampling
Delivery batch
Note: When the non-breakable ferroalloy is packaged for delivery, the minimum number of blocks to be sampled shall be increased by 50% according to Table 11. 6.4 Sampling method
6.4.1 Bulk collection
Accuracy of sampling
In a batch of goods, the number of sampling blocks shall be determined according to the maximum batch size of the ferroalloy (Table 11), and the sampling position shall be selected by random sampling method or systematic sampling method, and a piece of ferroalloy shall be picked up manually or smashed. The amount of sample taken from each piece shall meet the requirements of 6.2 and be roughly the same. 6.4.2 Sampling of packaged items
Packaged items are usually sampled by a two-step sampling method. During the sampling process, random sampling or systematic sampling can be used. When the number of pieces specified in Table 11 is not the same as the number of packages in the supply batch, at least one package that is alternating with the specified number of pieces shall be selected, and then one piece of alloy shall be taken from each selected package. When the number of pieces specified in Table 11 is the same as the number of packages in the supply batch, two or more pieces of alloy may be selected from each package, and the amount of gold and diamond taken from each piece shall be exactly the same and meet the requirements of .2. 6.5 Sample preparation method
6.5.1 Precision of sample preparation;
When the confidence level of the chemical composition of the supply is 95%, the precision of sample preparation is shown in Table 12. Table 12
Characteristic elements
Simple sample precision
Fec'rt. Not easy to break)
6.5.2, low, micro chromium iron and chromium nitride iron, metal chromium sample preparation method: C
Drilling points are randomly avoided when the sample is broken, and the edge of the drilling point should be 5mm or less away from the surface of the chromium iron ingot. During the drilling process, the drill bit should be cooled by running water. The drilling time should not be too long each time to prevent the sample from overheating and oxidation. The sample must be dried when it is wet, and the temperature should be controlled below 100℃. The dried sample is first sieved with a 0.151mm sieve to remove the sieved material-to remove foreign impurities. Or magnetic adsorption is used to remove foreign inclusions. The sample composed of graded batches should be ground, and the interval should not be more than 30s. The length of the sample after grinding is not more than 1.6mm. Mix well. Then reduce. The weight of each test sample for chemical analysis should not be less than 50.6.5.3 Sample preparation method for vacuum pin iron: First, soak each chrome iron brick in water, take it out and brush the surface with a steel brush to remove impurities. Then drill points of approximately equal weight on the diagonal lines of the vertical side of each brick at equal distances. The drilling depth is 1/2 of the whole brick. The sample is shaved into the steel container with a sharp steel brush, baked and mixed, and ground with a non-embedded tool so that it all passes through a 0.28rmm sieve. Then, weigh the same weight from the mixed sample of each brick, mix and divide. Note that the reduction must be carried out on a stainless steel plate. The weight of each test sample for chemical analysis should not be less than 50 g.
7 Sampling and preparation of ferrotitanium, ferromolybdenum, ferrotungsten, sawn iron, ferrovanadium, vanadium-aluminum alloy, rare earth ferrosilicon alloy, rare earth magnesium ferrosilicon alloy, molybdenum oxide block, sawn manganese ferroalloy
7.1 Comprehensive precision of the supplied chemical composition: When the supply chemical composition is reduced to 9, its comprehensive precision is shown in Table 13. 7.2 Sampling 7.2.1 Number of incremental samples GB/T 4010—94 10-98 0.89 FeSiRE FeSiMgRE 0.62 1 (h 62 The minimum number of incremental samples and the corresponding relationship between the rated maximum particle size of the batch of goods shall comply with the provisions of Table 14 in Length 11 Rated maximum particle size Number of incremental samples and sampling precision The minimum number of incremental samples and sampling precision shall comply with the provisions of Table 15. 7.2. 2-1
Delivery batch
Most refined
F+SiRE
FcSiRE
FeMnNh
FeSiMgkH FeM-Nl,
FeSiMgRE
Delivery batch
GB/T 4010—94
Continued Table 15
FeSiRE
FeSiMgRE
7.2.2.2 For ferrovanadium and vanadium-aluminum alloys, the minimum number of batches and sampling accuracy shall comply with the provisions of Table 16. Table 16
Delivery batch.t
7.2.3 Sampling method
Minimum number of batches
FeMnNb
Sampling accuracy Bs-%
For ferrotitanium, ferrotungsten, ferromolybdenum, ferrovanadium Iron, vanadium aluminum alloys, rare earth ferrosilicon alloys, rare earth magnesium ferrosilicon alloys, oxide blocks, niobium manganese ferrosilicon alloys, etc. are generally supplied in batch packaging. The sampling method usually adopts a two-step sampling method. Random sampling or systematic sampling can be used in the sampling process.
When the number of samples specified in Table 15 and Table 16 is less than the number of packages in the supply batch, at least the same number of packages as the number of samples should be selected, and one sample should be taken from each package. When the number of samples specified in Table 15 and Table 16 is greater than the number of packages supplied, 2 or 2 samples can be selected from each package. 7.2.3.1 When the rated maximum particle size is greater than 150 mm, the sample size can be taken manually by picking up or smashing it from the selected package. When the rated maximum particle size is not greater than 150 mm, the sample size can be taken manually by picking up or smashing it from the selected package with a sampling shovel that meets the requirements of Table 1 (the sample size can also be picked up manually). When the rated maximum particle size is not greater than 4 mm, the sample size can be taken manually by picking up the sample from the selected package with a sampling shovel that meets the requirements of 3.2. 7.2.3.2 When the particle size distribution in the package is quite different, the sample should be proportional to the particle size distribution in the package. 7.3 Sample preparation
7.3.1 Precision of sample preparation
When the confidence level of the supplied chemical composition is 95%, the precision of sample preparation is shown in Table 17. Table 17
Persistent elements
Sample preparation precisionB technology
FeSiRE
FeSiMgRE
GB/T 4010—94
7.3.2 After the sample is crushed, it is required to be sieved completely. According to the maximum particle size of the sample, the minimum sample amount left after reduction is determined. See Table 18.
Maximum particle size of the sample
FeTi F+Nh
Appendix; Preparation of FcTi test sample (example) Figure: Delivery quantity
Crushed to
Weight of sample after reduction
Crushed to -2.8mm
Weight of sample after reduction 0.8 kg
Crushed to -1.0mm
Weight of sample after reduction 300 g
Grinded to -0. 16 mm
Four test samples, each weighing 50 g
7.4 Test sample
Minimum weight after reduction, kg
FeMnFeW FeyAVYMaFesikEFesiMgREFeMnNh3.8
-10 mm
The rated maximum particle size is 100 mm
5kg×11
divided 3 times
divided 3 times
The weight of the test sample for chemical analysis should not be less than 50g. For all ferroalloys except ferrovanadium and vanadium-aluminum alloys, the particle size of the test sample should not exceed 0.16 mm, and the particle size of the test sample of ferrovanadium and vanadium-aluminum alloy should not exceed 11.25 mms. Note: The maximum particle size of the analytical sample should be developed according to the requirements of the corresponding separation method.
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