QB/T 2317-2012 English PDF (QBT2317-2012)

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QB/T 2317-2012: Oral care and cleansing products. Crude calcium carbonate for toothpaste
QB/T 2317-2012
NATIONAL LIGHT INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.40
Classification No.: Y43
Record No.: 36651-2012
Replacing QB/T 2317-2007
Oral Care and Cleaning Products -
Crude Calcium Carbonate 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 ... 5
2 Normative References ... 5
3 Requirements ... 6
4 Test Methods ... 7
5 Inspection Rules ... 19
6 Marking, Package, Transportation and Storage ... 20
Oral Care and Cleaning Products -
Crude Calcium Carbonate for Toothpaste
1 Scope
This Standard specifies the requirements, test methods, inspection rules and marking,
package, transportation, storage, shelf life of crude calcium carbonate for toothpaste.
This Standard is applicable to the crude calcium carbonate for toothpaste through
water washing, drying, and processed by Raymond mill.
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 document.
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
Method
GB/T 9724 Chemical Reagent - General Rule for the Determination of pH
GB/T 9735 Chemical Reagent - General Method for the Determination of Heavy
Metals
GB/T 610.1 Chemical Reagent - General Method for the Determination of Arsenic
GB 8372-2008 Toothpaste
GB/T 6678 General Principles for Sampling Chemical Products
GB/T 6682 Water for Analytical Laboratory Use - Specification and Test Methods
GB/T 8170 Rules of Rounding off for Numerical Values and Expression and
Judgement of Limiting Values
Staphylococcus aureus / g Must not be detected
3.3 Net content
The net content of the packaging commodities shall conform to the provisions of No.75
Order [2005] from General Administration of Quality Supervision, Inspection and
Quarantine.
4 Test Methods
Unless otherwise specified, the reagents and water used in this Standard shall be
analytical reagent and the Class-III water specified in GB/T 6682.
In this Standard, unless otherwise specified, the standard solution for titration analysis,
standard solution for impurity measurement, and the reagents and products used in
test methods shall be prepared as stipulated in GB/T 601, GB/T 602 and GB/T 603.
4.1 Appearance
Visually identify the appearance of the sample.
4.2 Fineness measurement
4.2.1 Instrument
4.2.1.1 Metallic standard sieve: pore diameter of 45µm (325 meshes).
4.2.1.2 Funnel.
4.2.1.3 Quantitative filter paper.
4.2.1.4 Oven: accuracy of ±2°C.
4.2.1.5 Balance: accuracy of 0.1g.
4.2.2 Operation procedure
Accurately take 10.0g of specimen into a pre-wetted-by-water metallic standard sieve
with a pore size of 45µm; use a small water flow to rinse the sample (the water shall
not be too large to prevent the splashing of the sample); meanwhile, tilt and rotate the
sieve body till there is no sieve residue passing through the sieve; then flush the
material retained on sieve to the funnel with filter paper [pre-dry to the constant weight
in the (105±2) °C oven] and filter. The filter residue together with the filter paper shall
be dried to the constant weight at the constant temperature of (105±2) °C.
4.2.3 Results expression
Where:
X2 – water absorption of 20g of sample, in mL;
V1 – liquid level reading of the water in the burette before titration, in mL;
V2 – liquid level reading of the water in the burette after titration, in mL.
The difference between the results of two parallel determinations is no greater than
0.02%, and take the arithmetic mean.
4.4 Volatile measurement
4.4.1 Instrument
4.4.1.1 Analytical balance: accuracy of 0.0001g.
4.4.1.2 Weighing bottle: 25mL.
4.4.1.3 Oven: accuracy of ±2°C.
4.4.2 Operation procedures
Use the constant-weight weighing bottle to take about 2g of specimen, accurate to
0.0001g; place into the oven; dry to the constant weight at (105±2) °C; cool off to the
room temperature for weighing.
The specimen after constant weight shall be stored for the measurement of calcium
carbonate content.
4.4.3 Results expression
Use the mass fraction to express the volatile content X3, which shall be calculated by
Formula (3):
Where:
X3 – volatile content, in %;
m1 – mass of weighing bottle and specimen before drying, in g;
m2 – mass of weighing bottle and specimen after drying, in g;
m –specimen mass, in g.
The difference between the results of two parallel determinations is no greater than
4.7.1.4 Triethanolamine: 1+2 solution (prepared to be fresh; store for up to two weeks).
4.7.1.5 Calcium carboxylic acid indicator: place the calcium carboxylic acid indicator
and sodium chloride in a mortar at a ratio of 1+99; mill thoroughly, mix evenly; then
place into a wide-mouthed bottle with ground stopper.
4.7.1.6 Ethylenediaminetetraacetic acid disodium salt (EDTA): 0.02mol/L.
4.7.2 Operation procedures
Accurately take 0.5g of calcium carbonate specimen that has reached constant weight
at (105±2) °C, accurate to 0.0001g; place into the beaker; firstly, use small amount to
water to wet; then slowly add 10mL~20mL of 1+1 hydrochloric acid solution to heat
and dissolve; after cooling off, transfer into 250mL volumetric flask; use distilled water
to dilute to the scale; after shaking well, use pipette to pipet 25mL of test solution into
a 250mL conical flask; successively add 20mL~30mL of water, 5mL of triethanolamine
solution, 10mL of sodium hydroxide solution; shake well when adding a test solution;
finally, add a small amount of calcium carboxylic acid indicator; use EDTA standard
titration solution to titrate till it is changed from wine red to pure blue; meanwhile, do
the blank test.
4.7.3 Results expression
Use mass fraction to express the calcium carbonate content X4, which shall be
calculated by Formula (4):
Where:
X4 – calcium carbonate content, in %;
c – concentration of EDTA standard titration solution, in mol/L;
V – volume of EDTA standard titration solution consumed by titration, in mL;
V0 - volume of EDTA standard titration solution consumed by blank titration, in mL;
m – specimen mass, in g;
0.100 – mass of calcium carbonate (expressed in g) which is equivalent to 1.00mL of
ethylenediaminetetraacetic acid disodium salt (EDTA) (1.000 mol/L), in g.
The difference between the results of two parallel determinations is no greater than
0.2%, and take the arithmetic mean as the measurement results.
4.9.1 Instrument
Xu-type carbonic acid analyzer (the inner diameter of the air outlet covering the lead
acetate test paper is required to be 14mm~16mm).
4.9.2 Reagents
4.9.2.1 Lead acetate.
4.9.2.2 Thioacetamide.
4.9.2.3 Pure aluminum sheet: content no less than 99.7%.
4.9.3 Operation procedures
4.9.3.1 Preparation of reagents
4.9.3.1.1 Preparation of lead acetate test paper: immerse the white chronic filter paper
into 10% lead acetate solution for 10min; take it out; dry in a hydrogen sulfide-free
atmosphere; cut it into small squares with...