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QB/T 2900-2012 English PDF (QBT2900-2012)

QB/T 2900-2012 English PDF (QBT2900-2012)

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QB/T 2900-2012: Oral care and cleansing products. Sodium lauryl sulfate for toothpaste

This standard specifies the classification, requirements, test methods, inspection rules and markings, packaging, transportation, storage, shelf life of sodium lauryl sulfate (abbreviated as K12). This standard applies to fatty alcohols prepared by hydrogenation of natural oils and fats (main components are C12~14 alcohols), sodium lauryl sulfate prepared by sulfurization and neutralization with sulfur trioxide, including powders, needles (grain), liquid products.
QB/T 2900-2012
LIGHT INDUSTRY STANDARD OF
THE PEOPLE REPUBLIC OF CHINA
ICS 71.100.40
Classification number: Y43
Filing number: 36654-2012
Replacing QB/T 2900-2007
Oral care and cleansing products - Sodium lauryl
sulfate for toothpaste
ISSUED ON: MAY 24, 2012
IMPLEMENTED ON: NOVEMBER 01, 2012
Issued by: Ministry of Industry and Information Technology of PRC
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Product classification ... 5
4 Requirements ... 5
5 Test methods ... 7
6 Inspection rules ... 18
7 Marking, packaging, transportation, storage, shelf life ... 20
Oral care and cleansing products - Sodium lauryl
sulfate for toothpaste
1 Scope
This standard specifies the classification, requirements, test methods, inspection rules and markings, packaging, transportation, storage, shelf life of sodium lauryl sulfate (abbreviated as K12).
This standard applies to fatty alcohols prepared by hydrogenation of natural oils and fats (main components are C12~14 alcohols), sodium lauryl sulfate prepared by sulfurization and neutralization with sulfur trioxide, including powders, needles (grain), liquid products.
2 Normative references
The following documents are essential to the application of this document. For the dated documents, only the versions with the dates indicated are applicable to this document; for the undated documents, only the latest version (including all the amendments) are applicable to this standard.
GB 191 Packaging - Pictorial marking for handling of goods
GB/T 601 Chemical reagent - Preparations of standard volumetric solutions GB/T 602 Chemical reagent - Preparations of standard solutions for
impurity
GB/T 603 Chemical reagent - Preparations of reagent solution for use in test GB/T 5173 Surface active agents - Detergents - Determination of anionic- active matter content - Direct two-phase titration procedure
GB/T 5009.74 Method for limit test of heavy metals in food additives
GB/T 5009.76 Determination of arsenic in food additives
GB/T 6368 Surface active agents - Determination of pH of aqueous solution - Potentiometric method
GB 8170 Rules of rounding off for numerical values and expression and
judgement of limiting values
GB/T 13173.1 Method of sample division for detergents
GB 6283-2008 Chemical products - Determination of water Karl Fischer
method (general method)
Ministry of Health of the People's Republic of China
The Second Pharmacopoeia of the People's Republic of China
JJF 1070-2005 Rules of metrological testing for net quantity of products in prepackages with fixed content
Order of the General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China [2005] No.75 "Measures for the Supervision and Management of Quantitative Packaging Commodity
Measurement?€?
3 Product classification
Sodium lauryl sulfate is divided into three types according to form: powder, needle (grain), liquid products.
Structural formula: CH3(CH2)nOSO3Na (main component n = 11)
Carbon chain distribution and odor evaluation shall be agreed by both parties. 4 Requirements
4.1 Identification (Method 1)
The identification reaction of sodium salt shall be shown by a 10% aqueous solution of sodium lauryl sulfate. (See Appendix III of Pharmacopoeia II of the People's Republic of China).
It shall be acidified by adding 10% aqueous solution of sodium lauryl sulfate and hydrochloric acid, boiling for 20 minutes under low heating, to show the identification reaction of sulfate through solution. (See Appendix III of the Pharmacopoeia II of the People's Republic of China).
Identification (Method 2)
Method principle: Use Fourier transform infrared spectrum for identification. Operation procedure: Refer to Appendix IVC Infrared Spectrophotometry of "The Pharmacopoeia II of the People's Republic of China"; the infrared
absorption spectrum of this product shall be consistent with that of the standard 5 Test methods
Unless otherwise specified in the analysis, it shall use analytical reagents and distilled water or water of equivalent purity.
The test solution, preparation, standard titration solution and impurity standard solution used in this standard shall be prepared in accordance with the provisions of GB/T 601, GB/T 602, GB/T 603, unless no other requirements are indicated.
5.1 Identification test
5.1.1 The identification reaction test of the development of sodium salt by 10% aqueous solution of sodium lauryl sulfate is carried out according to the method specified in Appendix III of the "Pharmacopoeia of the People's Republic of China".
5.1.2 A 10% aqueous solution of sodium lauryl sulfate is acidified with hydrochloric acid, then boiled for 20 minutes under low heat. The identification reaction test of the sulfate development is carried out according to the method specified in Appendix III of the "Pharmacopoeia of the People's Republic of China".
5.1.3 Refer to the Appendix IVC Infrared spectrophotometry in ?€?Pharmacopoeia II of the People's Republic of China", the infrared absorption spectrum of this product is consistent with that of the standard product.
5.2 Preparation of specimen
The laboratory samples of sodium lauryl sulfate are prepared and stored in accordance with the provisions of GB/T 13173.1.
5.3 Appearance
Carry out visual inspection under the condition of non-direct light. Compare with the standard requirements.
5.4 Determination of active content
Method 1: Subtractive method (arbitration method)
The content (w??) of the active substance in sodium lauryl sulfate is expressed by mass fraction; calculated by the formula (1) and formula (2) using the subtractive method:
Powder and needle (grain) products:
Where:
w5 - The total solid content of liquid product, %.
m1 - The mass of the sample after drying, in grams (g);
m2 - The mass of the sample before drying, in grams (g).
Method 2: Two-phase titration
It is performed according to GB/T 5173.
5.5 Determination of soluble matter content (w1) of petroleum ether
5.5.1 Reagents
a) Anhydrous sodium sulfate;
b) Ethanol: 95%;
c) Ethanol solution: 50%;
d) Petroleum ether, boiling range 30 ??C ~ 60 ??C, distillation residue shall be not more than 0.002% (mass fraction).
5.5.2 Instruments
a) Beaker: 400 mL;
b) Separatory funnel: 500 mL;
c) Conical bottle: 250 mL.
5.5.3 Operating procedures
Weigh 10 g of sample, accurate to 0.0001g, in a 400 mL beaker. Add 100 mL of water and 100 mL of 95% ethanol to dissolve the sample. Transfer the solution to a 500 mL separatory funnel. Use the 50% ethanol solution to wash the residue from the beaker into the separatory funnel, until the total volume is about 300 mL. Then add 50 mL of petroleum ether (boiling range 30 ??C ~ 60 ??C). Shake it for 30 s. Let it stand still for stratification. If necessary, add a small amount of 95% ethanol to break the emulsion.
Separate the lower alcoholic water phase and put it in another 500 mL
separatory funnel. Add 50 mL of petroleum ether (boiling range 30 ??C ~ 60 ??C) for extraction. Extract the alcoholic water phase alternately three times in this way.
Combine the petroleum ether layer separated by the three extractions in c) Suction filter bottle: 500 mL;
d) Quantitative filter paper: medium speed;
e) High temperature furnace: can control the temperature at (900 ?? 10) ??C f) Porcelain crucible: 30 mL.
5.6.3 Operating procedures
Weigh 1 g (3 g for liquid product) of sample, accurate to 0.0001 g, in a 250 mL tall beaker. For powdered product, add about 2 mL of water to wet it; then add 100 mL of 95% ethanol. For the liquid product, directly add 100 mL of 95% ethanol; stir it uniformly and then cover a watch glass. Put it in a 60 ??C ~ 70 ??C water bath and digest it for 1 h. Use a weighed (30 mL) 4# glass sand core crucible to filter it. Then use about 25 mL of warm 95% ethanol to rinse it. Drain it. Repeat rinsing and drainage as such for 3 times.
Then, use the mixed solution of 100 mL of heated and boiled water and 20 mL of (1:1) hydrochloric acid to dissolve the ethanol insoluble in batches and rinse the beaker and the filter crucible. Use a clean suction filter bottle to sequentially filter the solution and washing solution. Transfer it into another 250 mL tall beaker. Heat to boil it. Slowly add 15 mL of 10% barium chloride solution. Keep it slightly boiling for 30 min. While still hot, use medium-speed quantitative filter paper to filter it. Use hot distilled water to rinse it until the filtrate is free of chloride ions (check with silver nitrate solution). Put the filter paper and the sediment together in a dry and weighed porcelain crucible. Slowly heat to carbonize it. Then move it into a 900 ??C high temperature furnace and burn it for about 30 minutes, until the residue is completely white. Move the crucible into a desiccator to cool to normal temperature and weigh it.
The sodium sulfate content w6 in sodium lauryl sulfate is calculated by mass fraction and calculated according to formula (7):
Where:
w6 - The content of sodium sulfate in the sample, %;
m1 - The mass of the crucible with barium sulfate after burning, in grams (g); m2 - The mass of the empty crucible after burning, in grams (g);
m0 - The mass of the sample, in grams (g);
V - The volume of silver nitrate standard solution consumed in titration, in milliliter (mL);
m0 - The mass of the sample, in grams (g);
0.0585 - The millimolar mass of sodium chloride, in grams per millimolar (g/mmol).
The difference between the parallel determination results shall not exceed 0.03%.
5.8 Determination of moisture and volatile matter
5.8.1 Instruments
a) Weighing bottle: D60 mm x 30 mm;
b) Electric heating oven: The temperature can be controlled at (104 ?? 1) ??C; c) Desiccator: Effective desiccant (such as color-changing silica gel) inside. 5.8.2 Operating procedures
Weigh 1 g of powder and needle-shaped sample, accurate to 0.0001 g, in a dry and weighed weighing bottle (D60 mm x 30 mm) and spread it out. Place the weighing bottle in an oven at (104 ?? 1) ??C to bake it for 2 h. Take it out and put it in a desiccator. Cool it for 30 mm and weigh it. Repeatedly put into the oven for 30 min and cool and weigh it, until the difference between two successive weights is less than 0.001 g, which is regarded as constant weight.
The moisture and volatile matter w4 in sodium lauryl sulfate is expressed by mass fraction and calculated according to formula (9):
Where:
w4 - The moisture and volatile matter in the sample, %;
m1 - The mass of the weighing bottle and sample before drying, in grams (g); m2 - The mass of the weighing bottle and sample after drying, in grams (g); m0 - The mass of the sample, in grams (g).
The difference between the parallel determination results shall not exceed 0.2%. 5.9 Determination of moisture
water to dilute to the mark. Prepare it into a solution containing 5% sodium lauryl sulfate, which is used as the solution to be tested.
Turn on the power of the Kllett instrument. Inject deionized water into the colorimetric cell. Wipe it clean and put it into the colorimetric chamber. Adjust the knob to zero the galvanometer?€?s pointer. Drain the water in the colorimetric cell. Use the solution to be tested to wash it. Inject the solution to be tested. Wipe it clean and put it in the colorimetric cell chamber. The galvanometer?€?s pointer will turn around. Adjust the knob. The reading on the dial at this time is the Kllett color value of the sample.
The difference between the parallel determination results is not greater than 1. 5.13 Determination of foaming amount
5.13.1 Instruments
a) Thermostatic water-circulator bath, 1 set;
b) Roche foam tester, 1 set.
5.13.2 Preparation of test solution
Weigh 10 g of the sample (accurate to 0.01 g) in a 100 mL beaker. Meanwhile heat 1000 mL of distilled water to 40 ??C. First use a small amount of distilled water to dissolve the specimen. Pour the dissolved test solution into a 1000 mL porcelain cup. Wash the beaker several times. Finally pour the remaining distilled water into a 1000 mL porcelain cup. Gently stir it evenly. Put it in a 40 ??C constant temperature water bath for heat preservation, to be tested.
5.13.3 Measurement procedure
5.13.3.1 Preparation
Turn on the Thermostatic water-circulator bath connected to the graduated tube jacket of the Roche foam tester, to keep the foam meter at 40 ??C. First use a small amount of 40??C distilled water to rinse the inner wall of the graduated tube. Then use the test solution to rinse the wall. The rinsing operation must be complete. Inject the test solution pre-heated to 40 ??C from the lower end of the graduated tube. Adjust the liquid level of the test solution to the 50 mL scale. 5.13.3.2 The first test
Use a pipette to accurate take 200 mL of test solution. Then place it on the top of the graduated tube holder, to be perpendicular to the cross-section of the graduated tube, so that when the test solution flows in, it can reach the center of the liquid level in the graduated tube. Open the piston of the pipette, to make the test solution flow down all at once. When the test solution flows out, method, that is, after the test results are rounded off according to GB 8170 to the effective number of digits in accordance with the technical requirements, the test batch is judged as qualified or unqualified with reference to the limit values in the technical requirements.
If one of the physical-chemical index test results does not comply with the provisions of this standard, it is allowed to sample again from the double sample of the batch to retest the unqualified items. If it still fails, the batch of products is judged to be unqualified.
6.5 Arbitration
If both parties of the supplier and the purchaser have an objection to the product inspection results, the two parties can negotiate to resolve it. If necessary, they can jointly select an arbitration institution to inspect and rule according to this standard.
7 Marking, packaging, transportation, storage, shelf
life
7.1 Markings
Packaging bags, boxes or barrels shall have the following marks and comply with the provisions of GB 191:
a) Product name and grade;
b) Gross weight and net content;
c) Production batch number and packaging date;
d) Manufacturer name and site;
e) Product standard number;
f) Shelf life;
g) Text or signs on ?€?avoid rain?€?, ?€?avoid sun exposure?€?, ?€?avoid hooking?€?, etc., as well as restrictions on the number of stacking layers.
7.2 Packaging
The powder and needle (grain) products of sodium lauryl sulfate can be packed by polypropylene woven bag lined with plastic film, kraft paper three-in-one bag or cardboard box. The liquid products are packed in plastic drums or suitable metal drums. The actual net weight shall not be lower than the nominal mass.

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