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Similar standardsGB/T 28159-2011: Electronic grade phosphoric acid---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/GBT28159-2011GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 31.030 L 90 Electronic grade phosphoric acid Issued on: DECEMBER 30, 2011 Implemented on: JULY 01, 2012 Issued by. General Administration of Quality Supervision, Inspection and Quarantine; Standardization Administration of the People’s Republic of China. Table of ContentsForeword... 3 1 Scope... 4 2 Normative references... 4 3 Product categories... 5 4 Requirements... 5 5 Test methods... 6 5.1 Safety instructions... 6 5.2 General provisions... 6 5.3 Appearance... 6 5.4 Phosphoric acid content... 6 5.5 Readily oxidizable substance content... 7 5.6 Metal ion content... 7 5.7 Anion content... 10 5.8 Particle measurement... 15 6 Inspection rules... 15 6.1 Batching and sampling... 15 6.2 Inspection items... 16 7 Marking, labeling... 16 8 Packaging, transportation, storage and handling... 17 Appendix A (informative) Instrument working conditions... 18 Appendix B (informative) Ion chromatogram... 20 Electronic grade phosphoric acid1 ScopeThis Standard specifies the requirements, test methods, inspection rules, as well as marking, packaging, transportation, storage, etc. of electronic grade phosphoric acid. This Standard applies to electronic grade phosphoric acid for industry use. This Standard does not address safety issues in use. Users of this Standard are responsible for establishing appropriate safety and health clauses and limitations on the scope of use.2 Normative referencesThe following documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. GB/T 191, Packaging - Pictorial marking for handling of goods GB/T 601, Chemical reagent - Preparations of reference titration solutions GB/T 603, Chemical reagent - Preparations of reagent solutions for use in test methods GB/T 1282-1996, Chemical reagent - Phosphoric acid GB 3149-2004, Food additive - Phosphoric acid GB/T 6678, General principles for sampling chemical products GB/T 8170, Rules of rounding off for numerical values & expression and judgment of limiting values GB/T 11446.1, Electronic Grade Water GB 15258, General rules for preparation of precautionary label for chemicals GB 50472, Code for design of electronic industry clean room spectrometer separates the ions according to the mass-to-charge ratio and quantifies the content of the corresponding ions in the sample by the intensity of the ion mass spectrum peak. Use the standard addition method for sample analysis, and the linear range of the standard curve is 20 ng/L ~ 500 ng/L. 5.6.2 Reagents and materials 5.6.2.1 Nitric acid. Ultrapure nitric acid with a metal ion content not exceeding 1 μg/L, or a certified standard solution of the corresponding concentration. 5.6.2.2 Nitric acid solution (1+19, volume ratio). Take 150 mL of nitric acid as specified in 5.6.2.1 and add it to 950 mL of ultrapure water. 5.6.2.3 Tuning solution. 1 μg/L, provided by the instrument supplier or a certified tuning solution. 5.6.2.4 Tuning working solution. Take 20 mL of the tuning solution specified in 5.6.2.3 and place it in a clean polytetrafluoroethylene bottle. This solution can be kept for 7 days if refrigerated at 4 ℃ and used repeatedly. 5.6.2.5 Multi-element standard stock solution. Select the standard solution with a known metal ion concentration of 100 μg/mL listed in Table 1, or select a certified standard solution of other concentrations. 5.6.2.6 Multi-element standard working solution. Take 100 μL of the standard stock solution specified in 5.6.2.5 and place it in a clean polytetrafluoroethylene bottle; add 2 mL of nitric acid specified in 5.6.2.1; use ultrapure water to dilute to 100 mL; shake well. The metal ion concentration in this standard working solution is 100 μg/L. This solution can be kept for 7 days if refrigerated at 4 ℃ and used repeatedly. 5.6.2.7 High-purity argon, hydrogen, helium and other gases required by the instrument shall have a purity of not less than 99.995%. 5.6.2.8 Phosphoric acid standard sample (quality control sample). 1% phosphoric acid standard solution. Select a certified phosphoric acid standard solution or a quality control sample approved by inter-laboratory comparison. 5.6.3 Instruments and apparatuses 5.6.3.1 Inductively coupled plasma-mass spectrometer (ICP-MS), equipped with Collision Reaction System (ORS) (recommended instrument detection limit. low-mass elements (Be) < 5 × 10-9, medium- and high-mass elements (In, Bi) < 1 × 10-9; abundance sensitivity. low-mass elements ≤ 1 × 10-6, high-mass elements ≤ 5 × 10-7; stability. short-term RSD ≤ 4% (20 min), long-term RSD ≤ 5% (2 h), 24-hour mass axis deviation ±0.1 amu; anti-interference capability. oxide ratio ≤ 3%, double charge ratio ≤ 8%.) 5.6.3.2 Precision sampling gun. 100 μL, 1 000 μL, 5 mL. 5.6.3.3 Ultrapure water purifier, with a 0.1 μm terminal filter, for online preparation of ultrapure water with a purity of not less than 18.2 MΩ·cm (25 °C). 5.6.4 Analysis steps 5.6.4.1 Sample test fluid Weigh 10 g of the sample to be tested in batches to an accuracy of 0.000 2 g; place them in six 100 mL high-purity polytetrafluoroethylene bottles; add 2 mL of ultrapure nitric acid; then add 0 mL, 0.1 mL, 0.2 mL, 0.4 mL, 0.6 mL, and 1.0 mL of the multi-element standard working solution specified in 5.6.2.6 in that order; use ultrapure water to dilute to 100.00 g; shake well. 5.6.4.2 Blank test solution Add 2 mL of ultrapure nitric acid to a polytetrafluoroethylene high-purity bottle; use ultrapure water to dilute to 100 mL (100.00 g); shake well. All utensils and sampling gun tips must be soaked in high-purity nitric acid solution that meets the requirements of 5.6.2.2 for 24 hours, rinsed repeatedly with ultrapure water and dried before use. 5.6.4.3 Determination Adjust the instrument working conditions and use the tuning working solution specified in 5.6.2.4 to adjust the instrument measurement parameters. The tuning shall meet the instrument working requirements. Select the mass number of the element to be measured. The selection of the isotope of the element to be measured shall be based on the possible interference in the sample matrix. Select a suitable gas mode with less interference and determine the isotope with higher abundance. With the response value of the analytical peak as the ordinate and the amount of standard solution of the element to be measured as the abscissa, use the chemical workstation equipped with the instrument (random chromatography software) to draw a standard curve for the test results. The content corresponding to the distance between the intersection of the standard curve on the horizontal axis and the origin is the content of the element to be measured in the sample test solution. This is then used to calculate the content of the element to be measured in the sample. Carry out a blank test under the same analytical conditions; deduct blank interference according to the operating requirements of the instrument manual. The linear correlation coefficient of the standard curve shall not be lower than 0.995.If the measurement result exceeds the linear range, the test solution shall be re-prepared or the sample concentration shall be changed and re-measured. Note. When adjusting the instrument, it is advisable to give priority to comparative determination of phosphoric acid standard samples that meet the requirements of 5.6.2.8.The absolute difference between the determination results of the main elements and the known concentrations should not exceed a certain percentage limit (relative to the known concentration). Otherwise, the instrument should be readjusted. If the concentration of an element is known to be ≥1×10-7, the limit value is ≤10%; if the concentration of an element is known to be 1×10-8 ~ 5×10-98, the limit value is ≤20%; if the concentration of an element is known to be 1×10-9 ~ 1×10-8, the limit value is ≤30%. 5.6.5 Detection-limit, precision and recovery 5.6.5.1 Detection-limit (LOQ) The detection-limit of various elements in 1%H3PO4 are shown in Table A.1 in Appendix A. 5.6.5.2 Precision (RSD) The absolute difference between two independent determination results obtained under repeated conditions shall not exceed 30% of the arithmetic mean; the precision test data of each element are shown in Appendix A Table A.2. 5.6.5.3 Recovery The recovery of inductively coupled plasma-mass spectrometry shall be in the range of 75% ~ 125%; the test data of precision of each element are shown in Appendix A, Table A.2. 5.7 Anion content 5.7.1 Volumetric method Operated in accordance with the relevant requirements of GB/T 1282-1996, the detection-limit shall be ρ(Cl-) 0.01 mg/L, w(NO- 3) 0.05 mg/kg, ρ(SO2- 4) 0.4 mg/L. 5.7.1.1 Chloride 5.7.1.1.1 Reagents and materials a) Nitric acid. 1+1 solution; b) Silver nitrate. 17 g/L solution; c) Chloride standard solution [ρ(Cl-) = 1 000 mg/L]. select a certified standard solution of corresponding concentration. 5.7.1.1.2 Analysis steps Leave the solutions prepared according to a) and b) for 10 min. The turbidity of the solutions shall not be greater than that of the corresponding standard comparison solutions. 5.7.2 Ion chromatography (quantitative method) 5.7.2.1 Principle of the method The ion chromatograph uses a sample loop tube for fixed volume injection. The sample solution passes through a dedicated ion suppression column, and the trace impurity anions are separated from the phosphoric acid using an ion exclusion column. The separated and collected components are then concentrated through an ion exchange concentration column and form a Gaussian distribution chromatographic peak in the conductivity detector. The area (or peak height) of the chromatographic peak is proportional to the concentration of the component. The integrator of the instrument picks up this signal and gives the quantitative result of the component. The standard addition method should be used to determine the impurity anions in the sample. 5.7.2.2 Reagents and materials 5.7.2.2.1 Anion standard working solution Separately draw standard working solutions of chloride (Cl-), nitrate (NO- 3), and sulfate (SO2- 4) to prepare mixed standard working solutions of ρ(Cl-)10 mg/L, ρ(NO- 3) 50 mg/L and ρ(SO2- 4)100 mg/L. The appropriate concentration can be determined according to the anion concentration in the sample. 5.7.2.2.2 Ion chromatography columns Use ion chromatography columns supporting the instrument. guard column, analytical column, C concentration column, capture column and exclusion column. 5.7.2.2.3 Eluent Ultrapure water, 20 mmol/L ~ 60 mmol/L potassium hydroxide (preferably produced by an eluent generator). 5.7.2.3 Equipment and instruments Ion chromatograph, equipped with an automatic eluent generator, a conductivity detector and a chromatography workstation, an automatic anion regeneration suppressor, a concentration pump, and an external six-way valve. The instrument detection limit is. 0.002 μg/mL for Cl-, 0.001 μg/mL for NO- 3 and SO2- 4. 5.7.2.4 Analysis steps 5.7.2.4.1 Ion chromatography conditions 6.1.2 Sampling should be carried out online at the sampling port of the packaging machine on the production line. When sampling finished products, determine the number of sampling unit in accordance with the provisions of GB/T 6678.Before sampling, first confirm that the temperature of the product in the package is higher than 10 °C. Carry out sampling in a clean room at a room temperature of approximately 20 °C. The sampling method is to place the package in a Class 100 ultra-clean working environment (laminar flow hood or clean room) specified in GB 50472 for no less than 30 minutes; allow it to stabilize; then open the lid for sampling. When sampling, use a special clean sampler to insert it into the packaging barrel to three-quarters of the depth of the material layer to take samples. 6.1.3 When the sample is not less than 100 g, mix the sample evenly and divide it into two clean and dry high-purity polyethylene bottles or polytetrafluoroethylene bottles and seal them. Affix a label to the bottle, indicating. manufacturer name, product name, batch number, sampling date and name of the sampler (the label can be simplified if the manufacturer samples the product itself). Use one bottle for testing and keep the other for 3 months for future reference. 6.2 Inspection items 6.2.1 Factory inspection shall be carried out by the quality supervision and inspection department of the manufacturer in accordance with the requirements of this Standard. The manufacturer shall ensure that each batch of products leaving the factory complies with the requirements of this Standard. 6.2.2 When any of the following situations occurs, carry out type inspection. a) When there are major changes in raw materials, processes, or equipment; b) When resuming production after a long-term shutdown; c) When the quality supervision department makes a request.7 Marking, labeling7.1 The packaging drums of electronic grade phosphoric acid shall be firmly and clearly marked with the following information. manufacturer’s name and address, product name “electronic grade phosphoric acid”, production license number, net weight, batch number or production date, number of this standard, and the “corrosive article” mark specified in GB/T 191 and GB 15258.The label format shall comply with the provisions of GB 15258. 7.2 Each batch of electronic grade phosphoric acid shipped out of the factory shall be accompanied by a quality certificate. The contents shall include. manufacturer name, product name, net weight, batch number or production date, certification that the product quality complies with this Standard and a reference to this Standard. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. |
