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GB/T 13088-2006: Determination of chromium in feeds Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid GB/T 13088: Historical versions
Similar standardsGB/T 13088-2006: Determination of chromium in feeds---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT13088-2006GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 65.120 B 46 Replacing GB/T 13088-1991 Determination of chromium in feeds Issued on. JUNE 09, 2006 Implemented on. SEPTEMBER 01, 2006 Issued by. General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China; Standardization Administration of the People's Republic of China. Table of ContentsForeword... 3 1 Scope... 4 2 Normative references... 4 3 Method 1.Atomic absorption spectrometry... 4 4 Method 2.Spectrophotometry... 9ForewordThis Standard is a revision to GB/T 13088-1991 "Method for determination of chromium in feeds". Compared with GB/T 13088-1991, the main technical differences in this Standard are as follows. the atomic absorption spectrometry method for the determination of chromium in feed is added and determined as the arbitration method. At the same time, the original spectrophotometry is remained. This Standard replaces GB/T 13088-1991 from the date of implementation. This Standard was proposed by and shall be under the jurisdiction of National Technical Committee on Feed Industry of Standardization Administration of China. The drafting organizations of this Standard. Chinese Academy of Agricultural Sciences Animal Husbandry Research Institute, Chinese Academy of Agricultural Sciences Feed Research Institute. Main drafters of this Standard. Gu Xianhong, Li Wenying, Zhang Ping. Version of standard substituted by this Standard is. - GB/T 13088-1991. Determination of chromium in feeds1 ScopeThis Standard specifies two methods for the determination of chromium content in feed by atomic absorption spectrometer and spectrophotometer. Method 1 of this Standard is atomic absorption spectrometry. It is applicable to feed raw materials (including leather powder for feed, hydrolyzed leather powder), trace element premixes, compound premixes, concentrates and compound feeds. The minimum detection limit of graphite furnace atomic absorption spectrometry is 0.005 μg/kg. The minimum detection limit of flame atomic absorption spectrometry is 150 μg/kg. Method 2 of this Standard is spectrophotometric method. It is applicable to the determination of chromium in feed raw materials (including hydrolyzed leather powder) and compound feed.2 Normative referencesThe provisions in following documents become the provisions of this Standard through reference in this Standard. For dated references, the subsequent amendments (excluding corrigendum) or revisions do not apply to this Standard, however, parties who reach an agreement based on this Standard are encouraged to study if the latest versions of these documents are applicable. For undated references, the latest edition of the referenced document applies. GB/T 6682, Water for analytical laboratory use - Specification and test methods (neq ISO 3696) GB/T 14699.1, Feeding stuffs - Sampling 3 Method 1.Atomic absorption spectrometry 3.1 Principle The sample is ashed at high temperature. After dissolving with acid, inject it into the atomic absorption spectrometer detector. In a certain concentration range, its absorption value is proportional to the chromium content. Compare with the standard series to quantify. 3.2 Reagents and solutions Unless otherwise specified, the reagents used in Method 1 are guaranteed reagents; the water is ultrapure water or water of corresponding purity, which meets the requirements of GB/T 6682 for grade one water. 3.3 Instruments and equipment All glassware and crucibles are immersed in nitric acid solution (3.2.3) for 24 h or longer. User pure water to rinse. Dry in the air. 3.3.1 Experimental sample grinder or mortar (chromium-free). 3.3.2 Ultrapure water device (Millipore). 3.3.3 Analytical balance. resolution is 0.0001 g. 3.4 Specimen preparation According to GB/ T 14699.1, collect about 2 kg of representative feed raw materials (including leather powder for feed, hydrolyzed leather powder), mineral element premix, compound premix, concentrate and compound feed. Use quartering method to reduce it to about 250 g. Grind and pass through the 1 mm hole sieve. Mix well. Put in an airtight container. In order to prevent the specimen from deteriorating, it should be stored at low temperature for later use. 3.5 Analysis steps 3.5.1 Preparation of specimen solution Weigh 0.1 g ~ 10.0 g of specimen (accurate to 0.0001 g). Place in the 60 mL porcelain crucible. Perform complete carbonization on the electric furnace. Place in the muffle furnace. Starting from room temperature, gradually increase the temperature to 600°C for 5 h, until the specimen is white or off-white without carbon particles. 3.5.2.2 Standard curve drawing 3.5.2.2.1 Flame method Pipette 0.00 mL, 1.25 mL, 2.50 mL, 5.00 mL, 10.00 mL, 20.00 mL of chromium standard solution 1 (3.2.4.2). Respectively place them in 20 mL volumetric flasks. Add nitric acid solution (3.2.2) to dilute to the scale. Mix well. Make them standard working solutions. Each milliliter of solution in the volumetric flask is equivalent to 0.00 μg, 1.25 μg, 2.50 μg, 5.00 μg, 10.00 μg, and 20.00 μg of chromium, respectively. 3.6 Result calculation 3.6.1 Flame method The content X1 of chromium in feed, expressed in mass fraction micrograms per gram (μg/g), is calculated according to formula (1). 3.7 Repeatability The same analyst performs two measurements on the same specimen simultaneously or in rapid succession. The relative deviation of the obtained results. 4 Method 2.Spectrophotometry 4.1 Principle Decompose the sample by dry ashing. Chromium ions in it are oxidized to hexavalent chromium ions in alkaline potassium permanganate solution. Adjust the solution acidic again. Make hexavalent chromium ion (Cr6+) and diphenylcarbazide [(C6H5)2·(NH)4·CO] to generate rose red chromium compound. Perform colorimetric measurement. Calculate the chromium content. 4.2 Reagents and solutions Unless otherwise specified, the reagents used in this Method 2 are analytically pure; the water is distilled water or water of corresponding purity, which conforms to the provisions of GB/T 6682 for grade three water. 4.3 Instruments and equipment 4.3.1 Analytical balance. the resolution is 0.0001 g. 4.3.2 High temperature electric furnace (muffle furnace). 4.3.3 Experimental sample grinder or mortar. 4.3.4 Temperature-controlled electric hob. 600 W. 4.3.5 Volumetric flasks. 50 mL, 100 mL, 200 mL, 1000 mL. 4.3.6 Pipettes. 0.5 mL, 1.0 mL, 5.0 mL, 10.0 mL. 4.3.7 Transfer pipettes. 5 mL, 10 mL, 25 mL. 4.3.8 Erlenmeyer flask. 150 mL. 4.3.9 Short-necked funnel. 6 cm in diameter. 4.5 Determination steps 4.5.1 Specimen processing Weigh 1.0 g ~ 1.5 g of specimen (accurate to 0.0001 g). Place in a 60 mL porcelain crucible. After the carbonization in the temperature-controlled electric furnace is complete, place it in the muffle furnace. Starting from room temperature, gradually increase the temperature to 600°C for 5 h until the specimen is white or off-white without carbon particles. 4.6 Determination result The chromium content in feeds, expressed as mass fraction milligrams per kilogram (mg/kg), is calculated according to formula (3). 4.7 Repeatability The same analyst performs two measurements on the same specimen simultaneously or in rapid succession. The relative deviation of the obtained results. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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