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GB/T 36526-2018 English PDF

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GB/T 36526-2018: Test methods of industrial nitrocellulose
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Basic data

Standard ID: GB/T 36526-2018 (GB/T36526-2018)
Description (Translated English): Test methods of industrial nitrocellulose
Sector / Industry: National Standard (Recommended)
Classification of Chinese Standard: G15
Classification of International Standard: 71.100.01
Word Count Estimation: 39,354
Date of Issue: 2018-07-13
Date of Implementation: 2018-11-01
Quoted Standard: GB/T 308; GB/T 606; GB/T 622; GB/T 626; GB/T 628; GB/T 629; GB/T 665; GB/T 678; GB/T 679; GB/T 684; GB/T 686; GB/T 687; GB/T 2306; GB/T 4202; GB/T 4895; GB/T 6682; GB/T 6684; GB/T 12589; GB/T 12591; GB/T 15349; HG/T 2765.4; HG/T 3438; HG/T 3449
Regulation (derived from): National Standard Announcement No. 10 of 2018
Issuing agency(ies): State Administration for Market Regulation, China National Standardization Administration
Summary: This standard specifies the nitrogen content, ash, moisture, humectant, viscosity, light transmittance, whiteness, color, acidity, stability, ignition point, cellar solubility of industrial nitrocellulose (hereinafter referred to as nitrocellulose). , plasticizer content, turbidity test methods of 14 kinds of test methods, reagents and materials, equipment, test procedures, test results processing, test reports and so on. The 14 test methods in this standard are applicable to the testing of nitrocellulose for coatings, inks, celluloids, household chemicals, environmentally friendly products, biomedical products, etc. The following methods are used for: 2) nitrogen content test The method includes three test methods: Divald alloy reduction method, interferometer method and near-infrared spectroscopy method. Divalde alloy reduction method is arbitration method, and interferometer method is common test method for production.

GB/T 36526-2018: Test methods of industrial nitrocellulose

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Test methods of industrial nitrocellulose ICS 71.100.01 G15 National Standards of People's Republic of China Industrial nitrocellulose test method Published on.2018-07-13 2018-11-01 implementation State market supervision and administration China National Standardization Administration issued

Content

Foreword III 1 Scope 1 2 Normative references 1 3 Terms and Definitions 2 4 nitrogen content test method 4 4.1 Diwald alloy reduction method 4 4.2 Interferometer method 7 4.3 Near Infrared Spectroscopy 9 5 ash test method 10 6 Moisture Test Method 11 6.1 Karl Fischer reagent method 11 6.2 Near Infrared Spectroscopy 13 7 humectant test method 14 8 Viscosity test method 15 9 Transmittance test method 20 10 Whiteness Test Method 22 11 Chroma test method 23 12 Acidity Test Method 24 13 Stability test method 26 14 Fire Point Test Method 30 15 Cellulose Solubility Test Method 31 16 Plasticizer content test method 33 17 Turbidity test method 34 Appendix A (informative) Industrial nitrocellulose test report 36

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009. Please note that some of the contents of this document may involve patents. The issuing organization of this document is not responsible for identifying these patents. This standard is proposed and managed by China Ordnance Industry Group Corporation. This standard was drafted. Sichuan Northern Nitrocellulose Co., Ltd., China Ordnance Industry Standardization Institute, China Ordnance Industry No. 2 The Fourth Institute, Beijing Institute of Technology. The main drafters of this standard. Zhang Renxu, Mai Lubo, Zhang Wei, Shao Ziqiang, Zhao Libin, Liu Hongni, Zhang Wei, Su Pengfei, Du Ying, Wang Wenjun, Ma Jun, Wen Xiaoyan, Liu Yanhua, Xu Hui, Shi Yan, Yue Lu. Industrial nitrocellulose test method Caution - Personnel using this standard should have practical experience in formal laboratory work. This standard does not indicate all possible security questions. question. It is the responsibility of the user to take appropriate safety and health measures and to ensure compliance with the conditions set by the relevant national regulations.

1 Scope

This standard specifies the nitrogen content, ash, moisture, humectant, viscosity, light transmittance of industrial nitrocellulose (hereinafter referred to as nitrocellulose). Whiteness, color, acidity, stability, ignition point, cellar solubility, plasticizer content, turbidity, 14 test methods, reagents and materials Materials, equipment, test procedures, test results processing, test reports, etc. The 14 test methods in this standard are applicable to coatings, inks, celluloids, daily chemical products, environmentally friendly products, biomedical products, etc. The test of nitrocellulose, in which the following methods are used. a) Test methods for nitrogen content include three test methods. Divald alloy reduction method, interferometer method and near-infrared spectroscopy, Divald The alloy reduction method is an arbitration method, the interferometer method is a commonly used test method, and the near-infrared spectroscopy method is a quick and simple test method; b) Moisture test methods include Karl Fischer reagent method and near-infrared spectroscopy method, Karl Fischer reagent method for arbitration Trial method, near infrared spectroscopy is a quick and easy test method; c) The humectant test method includes two methods. oven method and halogen lamp method. The oven method is the arbitration test method, and the halogen lamp method is fast and simple. Test method d) The viscosity test method includes two methods. falling ball viscosity method and capillary viscosity method. The falling ball viscosity method is suitable for conventional viscosity (viscosity is lower than 11.5mPa·s) nitrocellulose test, capillary viscosity method suitable for high viscosity (viscosity higher than 11.5mPa·s) nitrocellulose Testing e) The light transmittance test method includes two methods. acetone solvent method and mixed solvent method, and acetone solvent method is suitable for low nitrogen content (nitrogen content is 10.7%~11.3%) High-viscosity nitrocellulose transmittance test, mixed solvent method suitable for conventional viscosity nitrocellulose Rate test f) Stability test methods include Beckman Ronke method and Abel method. Beckman Ronke method is 132 °C heat resistance test Test method, Abel is 80 ° C heat test.

2 Normative references

The following documents are indispensable for the application of this document. For dated references, only dated versions apply to this article. Pieces. For undated references, the latest edition (including all amendments) applies to this document. GB/T 308 rolling bearing steel ball GB/T 606 General method for moisture determination of chemical reagents Karl Fischer method GB/T 622 chemical reagent hydrochloric acid GB/T 626 chemical reagent nitric acid GB/T 628 chemical reagent boric acid GB/T 629 chemical reagent sodium hydroxide GB/T 665 chemical reagent copper sulfate (II) sulfate (copper sulfate) GB/T 678 chemical reagent ethanol (anhydrous ethanol) GB/T 679 chemical reagent ethanol (95%) GB/T 684 chemical reagent toluene GB/T 686 chemical reagent acetone GB/T 687 chemical reagent glycerol GB/T 2306 chemical reagent potassium hydroxide GB/T 4202 fiberglass GB/T 4895 synthetic camphor GB/T 6682 Analytical laboratory water specifications and test methods GB/T 6684 chemical reagent 30% hydrogen peroxide GB/T 12589 Chemical reagent ethyl acetate GB/T 12591 chemical reagent ether GB/T 15349 chemical reagent bromocresol green HG/T 2765.4 blue glue indicator HG/T 3438 chemical reagent nitrogen fixed alloy HG/T 3449 Chemical Reagent Methyl Red HG/T 3498 chemical reagent butyl acetate HG/T 4101 chemical reagent phenolphthalein HG/T 4120 Industrial Calcium Hydroxide WJ255 Abel test with potassium iodide starch test paper manufacturing and acceptance technical conditions

3 Terms and definitions

The following terms and definitions apply to this document. 3.1 Industrial nitrocellulose industrialnitrocelulose Nitrocellulose used in coatings, inks, celluloids, daily chemical products, environmentally friendly products, biomedical products, etc. 3.2 Calibration model calibrationmodel A mathematical model of the relationship between the near-infrared spectrum of the sample and the corresponding reference value. 3.3 Prediction standard error standarderrorofprediction; SEP In the multivariate calibration, the prediction ability of the calibration model is evaluated, and the standard error calculated by verifying the sample standard value and the predicted value is used. press Equation (1) is calculated. SEP= i=1 (νi-νi)2 (1) In the formula. SEP---predicting standard error; Νi --- the predicted value obtained from the ith verification sample; Νi --- the standard value of the ith verification sample; m ---Verify the number of samples. 3.4 Calibration standard error standarderrorofcalibration; SEC In the multivariate calibration model, the prediction ability of the calibration model is evaluated, and the standard error calculated by correcting the sample standard value and the predicted value is used. Calculated according to formula (2). SEC= i=1 (yi-yi)2 (2) In the formula. SEC---corrected standard error; Yi --- the predicted value obtained from the ith corrected sample; Yi --- the standard value of the i-th calibration sample; d --- The degree of freedom of the calibration model (d is equal to nk, where n is the number of calibration samples and k is the number of model variables). 3.5 Mahalanobisdistance The covariance of the similarity of two unknown sample sets. Calculated according to formula (3). Hi= (ti-T)M-1(ti-T)' T= i=1 Ti M = (TT)'(TT) N-1 Ïï (3) In the formula. Hi --- covariance of Markov distance data; Ti --- calibration set sample i spectral score; T --- correction set average score matrix of n sample spectra; M --- Markov matrix of the calibration set sample; n --- the number of samples; T --- calibration set sample spectral score matrix. 3.6 Mahalanobisdistancelimitationvalue Calculated according to formula (4). HL=H 3SDMD (4) In the formula. HL --- Mahalanobis distance threshold; H --- The average value of the Markov distance of the calibration set sample; SDMD---The standard deviation of the Markov distance of the calibration set sample. 3.7 Abnormal sample abnormalsample The Mahalanobis distance is greater than the Mahalanobis distance threshold and exceeds the sample that corrects the analytical capabilities of the model.

4 nitrogen content test method

4.1 Divald alloy reduction method 4.1.1 Test principle Nitrocellulose is saponified with sodium hydroxide in the presence of hydrogen peroxide to form nitrates, which are reduced to ammonia by Divald alloy. Gas, condensed with water vapor, and absorbed by excess boric acid solution, using bromocresol green-methyl red as indicator, titration with hydrochloric acid standard solution Calculate the nitrogen content in the sample. 4.1.2 Reagents and materials 4.1.2.1 Water, Class III, GB/T 6682. 4.1.2.2 30% hydrogen peroxide, analytical grade, GB/T 6684. 4.1.2.3 Divald alloy (Cu. 50%, Al. 45%, Zn. 5%), HG/T 3438. 4.1.2.4 Ethanol, analytical grade, GB/T 679. 4.1.2.5 Boric acid solution. boric acid, analytically pure, GB/T 628, a solution with a mass fraction of 4%. 4.1.2.6 Sodium hydroxide solution. Sodium hydroxide, analytically pure, GB/T 629, a solution with a mass fraction of 20%. 4.1.2.7 Hydrochloric acid standard solution. hydrochloric acid, analytically pure, GB/T 622, concentration 0.2mol/L. 4.1.2.8 Bromocresol green, analytical grade, GB/T 15349. 4.1.2.9 Methyl red, analytically pure, HG/T 3449. 4.1.3 Equipment 4.1.3.1 Automatic tester for nitrogen content of nitrocellulose, mainly by microcomputer controller, steam generator, distillation system, boric acid system, dripping Composition system, waste disposal system and cleaning system, with automatic completion of reagent quantitative addition, distillation, absorption, titration and output test results Function, its schematic diagram is shown in Figure 1. 4.1.3.2 Porous saponification apparatus, the pore temperature should be adjustable from room temperature to 400 °C. 4.1.3.3 Analytical balance with an accuracy of 0.0001g. 4.1.3.4 The oven has a temperature control accuracy of ±2 °C. 4.1.3.5 Saponification tube, the specification is 250mL. 4.1.3.6 Dryer. 4.1.3.7 Weighing bottles. 4.1.3.8 Beakers, specifications are. 100mL, 1000mL. 4.1.3.9 Measuring cylinders, the specifications are. 5mL, 50mL. 4.1.3.10 Glass rods. Description. 1 --- operation panel; 9 --- standard hydrochloric acid barrel; 2 --- condensate tube; 10---boric acid barrel; 3 --- plus boric acid pipette; 11 --- distilled bucket; 4 --- plus hydrochloric acid standard solution tube; 12 --- saponification tube; 5 --- absorption bottle; 13---steam tube; 6 --- power switch; 14 --- sealed handle; 7 --- optical sensor; 15--- front cover (with distiller and condenser inside). 8 --- tray; Figure 1 Schematic diagram of automatic tester for nitrogen content of nitrocellulose 4.1.4 Test preparation 4.1.4.1 Preparation of equipment 4.1.4.1.1 Add the corresponding solution to each solution tank of the instrument so that the amount of the added solution meets the experimental requirements. 4.1.4.1.2 In order to ensure accurate test results, two or three blank tests are performed after each power-on, for instrument preheating and cleaning instruments. Pipeline. 4.1.4.2 Indicator preparation 4.1.4.2.1 Mixed indicator. bromocresol green is formulated into a 1g/L ethanol solution; methyl red is formulated to a concentration of 1g/L Ethanol solution; the bromocresol green ethanol solution and the methyl red ethanol solution were mixed at a volume ratio of 5.1. 4.1.4.2.2 Boric acid absorption solution. Add the mixed indicator (4.1.4.2.1) to the boric acid solution (4.1.2.5), mix, boric acid and mixed indicator The volume ratio is 100.1, placed in a cool place, and the storage period is one month. 4.1.4.3 Preparation of samples Use a pair of tweezers to tear the sample, and then take 1.5 times the required mass into the aluminum box. If it is an aqueous sample, it should be placed in an oven at 108 °C~ Dry at 112 ° C for 1 h, put it in a desiccator and cool to room temperature, then dry it again in an oven for 30 min, until the two samples are weighed twice. The difference is no more than 0.0005g. If it is an alcohol-containing sample, it should be placed in an oven at 100~105 °C for 1 hour, and placed in a desiccator to cool to the room. The temperature was then dried again in an oven for 30 minutes until the difference between the two sample samples did not exceed 0.0005 g. Known quality Weigh the bottle and weigh 0.40g~0.65g, accurate to 0.0001g. 4.1.5 Test procedure 4.1.5.1 Blank test 4.1.5.1.1 50 mL of distilled water was placed in a saponified tube pre-filled with 5 mL of ethanol. 4.1.5.1.2 Insert a funnel into the saponification tube, and add about 1.5mL~2mL of hydrogen peroxide solution and 50mL of sodium hydroxide solution. Shake well. 4.1.5.1.3 After 5min~10min, slowly heat on the graphite furnace saponifier, the heating temperature is about 150 °C, until the small bubble disappears Lose, cool the saponification tube to room temperature. 4.1.5.1.4 Quickly add 4g of Divald alloy to the saponification tube and immediately install the saponification tube on the instrument and seal it. hit Turn on the instrument steam switch, so that a small amount of steam flow is gradually heated, the recording time is about 30s, the steam switch is turned off, and the reaction is 10 minutes. 4.1.5.1.5 Start the instrument program, the instrument setting parameters should be. steam flow 80%, boric acid volume 35mL, distillation time 8min. The instrument simultaneously performs the steps of distillation, absorption, and titration, and titrates with a hydrochloric acid standard solution to obtain a titration result. 4.1.5.1.6 Perform the parallel blank test according to the procedure of 4.1.5.1.1~4.1.5.1.5. The difference between the two values should not exceed 0.05mL, and the average value should be taken. As a blank volume V0 of hydrochloric acid. 4.1.5.2 Sample test 4.1.5.2.1 Prepare two samples and perform two tests in parallel. 4.1.5.2.2 Pour the constant weight sample in the weighing bottle into a saponification tube containing 5 mL of ethanol, and divide the weighing bottle with 50 mL of distilled water. The washing was washed three to five times, and the washed distilled water was poured into a saponification tube. 4.1.5.2.3 Press 4.1.5.1.2. 4.1.5.2.4 After placing for 5min~10min, slowly heat the saponification on the graphite furnace saponifier. At this time, it should be shaken continuously until the sample solution changes. To clarify, the solution is clarified and heating is continued to destroy excess hydrogen peroxide until the small bubbles disappear. After the saponification reaction is completed, the saponification tube is cooled. To room temperature. 4.1.5.2.5 Repeat the operation according to 4.1.5.1.4 and 4.1.5.1.5. 4.1.6 Treatment of test results 4.1.6.1 The nitrogen content of nitrocellulose is calculated according to formula (5). wN= c(V-V0)×0.0140 m × 100 (5) In the formula. wN --- mass fraction of nitrogen content of nitrocellulose, %; c --- hydrochloric acid standard titration solution concentration value, the unit is mole per liter (mol/L); V --- sample consumption of hydrochloric acid standard titration solution volume value in milliliters (mL); V0 --- blank test consumption of the standard volume of hydrochloric acid titration solution, the unit is milliliter (mL); 0.0140---The value of the mass of nitrogen equivalent to 1.00mL hydrochloric acid standard titration solution (hydrochloric acid concentration 1.000mol/L), single The position is gram per millimol (g/mmol); m --- The value of the sample mass in grams (g). 4.1.6.2 The difference between the two parallel test calculation results should be no more than 0.04%, and the average value should be taken as the nitrogen content of nitrocellulose. Show to two decimal places. Retest when the calculated result difference is greater than 0.04%. 4.1.7 Test report See Appendix A for the content and format of the test report. 4.2 Interferometer method 4.2.1 Test principle The quantitative sample is taken in a special steel cylinder, and the sample is detonated by electric heating in the case of airtightness. Pass the blasted gas into the interferometer and measure it The number of interference fringes corresponding to the refractive index of the gas is determined from the reference curve, and the nitrogen content is calculated. 4.2.2 Reagents and materials 4.2.2.1 Copper sulfate pentahydrate, analytical grade, GB/T 665. 4.2.2.2 Color changing silica gel, HG/T 2765.4. 4.2.2.3 Soda lime. calcium hydroxide, HG/T 4120, 75%; water 20%; sodium hydroxide, GB/T 629, 3%; potassium hydroxide, GB/T 2306, 2% mixture. 4.2.3 Equipment 4.2.3.1 Interferometer, measuring tube length is 1000mm or 500mm, and its attached device, its structural schematic is shown in Figure 2. 4.2.3.2 Special steel cylinder (according to safety requirements), the material is stainless steel, the volume is about 300mL. 4.2.3.3 Nickel-chromium wire, diameter from about 0.1mm to 0.2mm. 4.2.3.4 Weighing shovel, made of aluminum or copper. 4.2.3.5 Dryer. 4.2.3.6 Aluminum box. 4.2.3.7 Thermometer, measuring range is 0 °C ~ 50 °C, the division value is 0.1 °C. 4.2.3.8 Barometer. 4.2.3.9 Ignition device, the working voltage range is 0V~20V, and the working current range is 0A~5A. 4.2.3.10 Water jet or vacuum pump. 4.2.3.11 Hair dryer. Description. 1, 3---silicone drying tube; 2 --- soda lime absorption; 4 --- microporous sintered plate filter; 5 --- Interferometer gas chamber standard tube inlet; 6 --- Interferometer chamber measuring tube inlet; 7 --- Interferometer gas chamber standard tube; 8 --- Interferometer gas chamber measuring tube; 9 --- filter, see loading glass wool; 10 --- acid ketone absorption tower, the bottom layer of flat glass wool (cloth), evenly spread on top a fixed thickness of anhydrous sodium sulfate; 11 --- Interferometer gas chamber measuring tube outlet; 12 --- Interferometer gas chamber standard tube outlet; 13 --- Thermometer insulation cover; 14 --- Rotameter. Figure 2 Schematic diagram of the interferometer and its attached devices 4.2.4 Test preparation 4.2.4.1 Sample Preparation Use a pair of tweezers to tear the sample, and then take 1.5 times the required mass into the aluminum box. If it is an aqueous sample, it should be placed in an oven at 108 ° C ~ 112 ° C. Dry for 1h, put it in a desiccator and cool to room temperature for later use; if it is an alcohol-containing sample, it should be placed in an oven at 100 ° C ~ 105 ° C for 1 h, put Cool to room temperature in a desiccator and set aside. 4.2.4.2 Instrument preparation 4.2.4.2.1 Rinse the special cylinder cylinder with water, wipe off the water drops, blow dry with a hair dryer or dry in an oven, wipe the special steel cylinder cover and blow it. Dry, set the rubber ring, and connect the resistance wire for use. 4.2.4.2.2 Disconnect the connecting hose between the insulation sleeve and the flowmeter, ......
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