FOR COMMENT ONLY PROPOSAL FOR A TRINIDAD AND TOBAGO STANDARD COMPULSORY DETERGENT – SYNTHETIC LAUNDRY DETERGENT POWDER – SPECIFICATION PCTTS 466: 20XX (1 st Revision) Date of Issue: Closing Date for Comments: 2009-06-08 2009-08-06 Send Comments to: The Executive Director, TRINIDAD AND TOBAGO BUREAU OF STANDARDS Century Drive, Trincity Industrial Estate, Macoya, TUNAPUNA P.O. Box 467, PORT OF SPAIN, Trinidad and Tobago Telephone: 662-8827, 662-3810, 663-4835/6 Telefax: 663-4335; E-mail: [email protected]
The Trinidad and Tobago Bureau of Standards (the Bureau) is a body corporate established under the authority of the Standards Act No. 18 of 1997 (herein after referred to as the Standards Act).
In accordance with the Standards Act, the Bureau shall promote and encourage the development and maintenance of standards and further shall establish standards for the following: to improve goods produced or used in Trinidad and Tobago; to ensure industrial efficiency and development; to promote public and industrial welfare, health and safety; and to protect the environment.
The Bureau develops standards through consultation with relevant interest groups, and public comment is invited on all draft standards before they are declared as Trinidad and Tobago Standards in accordance with the provisions of the Standards Act.
The Bureau is the legal custodian of Trinidad and Tobago Standard Marks, which are issued in accordance with the Standards Act. When a Trinidad and Tobago Standard Mark appears on any product, or in connection with any service, process or practice, it provides assurance that such a product, service, process or practice conforms to a Trinidad and Tobago Standard.
The Bureau’s Standards Information Centre maintains a reference library of standards, including local, regional and international standards and is the national node of the International Organization for Standardization Information Network (ISONET). The Centre also acts as the sales agent for the publications of foreign and international standards organizations.
NOTE In order to keep abreast of progress in the industries concerned, Trinidad and Tobago Standards are subject to periodic review. Suggestions for improvements are welcome.
PCTTS 466: 20XX
iv
AMENDMENTS ISSUED SINCE LAST PUBLICATION
AMENDMENT NO. DATE OF ISSUE TEXT AFFECTED
PCTTS 466: 20XX
v
ATTACHMENT PAGE FOR TTBS AMENDMENT SHEET
PCTTS 466: 20XX
vi
TRINIDAD AND TOBAGO STANDARD
DETERGENT – SYNTHETIC LAUNDRY DETERGENT POWDER –
SPECIFICATION
(1st Revision) ___________________________________________________________________________________ The Committee responsible for the development of this Trinidad and Tobago Standard is as follows:
Specification Committee for synthetic laundry detergent powder
Members Representing
Ms Denrica Christopher (Chairperson) Ministry of Legal Affairs, Consumer Affairs
Division Mr Douglas Clarke Hi Lo Food Stores Ms Vidia Persad Doodnath Trinidad and Tobago Manufacturers' Association Mr Damian George Genethics Pharmaceuticals Limited Mr Vivian George Ministry of Health, Chemistry, Food and Drugs
Division Mr Alexei Nimblett Caribbean Industrial Research Institute Mr Ramon O'Brien Unilever Caribbean Limited Mr Ryan Sooklalsingh Alstons Marketing Company Limited Ms Karlene Lewis Trinidad and Tobago Bureau of Standards, Laboratory Services Division Ms Reesa Thomas Trinidad and Tobago Bureau of Standards, Implementation Division Mr Sheva Serrattan (Technical Secretary) Trinidad and Tobago Bureau of Standards, Standardization Division
PCTTS 466: 20XX
vii
Contents
Foreword ........................................................................................................................................................... 1 Introduction ....................................................................................................................................................... 2 1 Scope ................................................................................................................................................... 3 2 Normative references ........................................................................................................................... 3 3 Terms and definitions ........................................................................................................................... 4 4 Requirements ....................................................................................................................................... 6 4.1 General requirements ........................................................................................................................... 6 4.2 Specific requirements ........................................................................................................................... 7 5 Test methods........................................................................................................................................ 9 6 Sampling .............................................................................................................................................. 9 6.1 Sample size.......................................................................................................................................... 9 6.2 Selection of primary packages.............................................................................................................. 9 6.3 Selection of secondary packages ....................................................................................................... 10 7 Conformity requirements .................................................................................................................... 10 7.1 Lot conformity ..................................................................................................................................... 10 7.2 Conformity assessment ...................................................................................................................... 10 8 Packaging and labelling...................................................................................................................... 11 Annex A (normative) Determination of moisture and volatile matter content................................................... 12 Annex B (normative) Determination of pH value............................................................................................. 13 Annex C (normative) Determination of matter insoluble in water .................................................................... 14 Annex D (normative) Determination of free alkali as NaOH............................................................................ 16 Annex E (normative) Determination of net weight of product.......................................................................... 17 Annex F (informative) Additional commonly used detergent ingredients ......................................................... 18 Tables
Table 1 — Chemical and physical requirements .............................................................................................. 8 Table 2 — Scale of sampling............................................................................................................................ 9
PCTTS 466: 20XX
viii
(This page was intentionally left blank)
PCTTS 466: 20XX
1
Foreword
This specification was declared a Trinidad and Tobago Standard on ………….., after the draft had been approved by the Trinidad and Tobago Bureau of Standards. This standard is a revision of TTS 466: 2002 – Detergent – Synthetic laundry detergent powder – Specification.
This standard was revised to reflect the new format of Trinidad and Tobago standards and to keep abreast with current practices in the industry. This first revision differs from the original standard as follows:
a) performance requirements have been removed; and
b) labelling requirements have been modified.
The Trinidad and Tobago Bureau of Standards has recommended that this standard be declared a compulsory standard to protect the consumer or user against danger to health or safety.
This revision will become effective as a compulsory standard on a date to be notified by the Minister responsible for trade and industrial development in a Notice to be published in the Trinidad and Tobago Gazette, as required by the Standards Act.
This national standard was developed for compliance by manufacturers, importers and distributors of synthetic laundry detergent powder.
In formulating this standard considerable assistance was derived from the following publication which was still current when this standard was being developed:
Annexes A, B, C, D, and E form a normative part of this standard. Annex F forms an informative part of this standard.
Annex A outlines the procedure to determine moisture and volatile matter content.
Annex B outlines the procedure to determine pH value.
Annex C outlines the procedure to determine matter insoluble in water.
Annex D outlines the procedure to determine the free alkali as sodium hydroxide.
Annex E outlines the procedure to determine net weight.
Annex F lists commonly used detergent ingredients.
PCTTS 466: 20XX
2
Introduction
Synthetic laundry detergent powder is a commonly used product in Trinidad and Tobago. It is customarily used for laundering by manual means or using automatic washing machines. Automatic washing machines include traditional agitator washers in which the textiles or fabrics are completely submerged in water while an agitator moves the laundry back and forth to dislodge soils. In most cases, traditional agitator washers are top-loading. Synthetic laundry detergent powder is typically formulated to be used in agitator washers. A considerable amount of water is required for the detergent to perform the functions of removing and preventing the redeposition of soils.
Due to increased environmental awareness, there is a need for more efficient detergents with a decreased environmental impact. Recent technological advances have led to the development of more efficient and environmentally friendly washers known as high efficiency washing machines. These washers are designed on the principle of a moving drum which creates a gentle tumbling motion of the laundry to dislodge the soils. High efficiency washers can be either front-loading or top-loading and all front-loading washers are high efficiency.
High efficiency detergents have been designed for use in these high efficiency washing machines. High efficiency washing machines utilize less water in their wash and rinse cycles and are relatively more energy efficient. High efficiency detergents are formulated to be compatible with high efficiency washing machines by producing reduced suds and by being more water-soluble. High efficiency detergents are typically available in the liquid form and are not covered by this standard.
This standard is intended to specify requirements for laundry detergent powder that is generally used in traditional agitator washing machines. Laundry detergent powder is not easily dissolved in high efficiency washing machines because such detergents require more water than the volume that is used in high efficiency washing machines. Traditional detergents also require higher volumes of water to prevent redeposition of soils, and excess suds production associated with these detergents can deter the mechanical operation of high efficiency washing machines. Ultimately, powdered laundry detergent is typically not formulated for use in high efficiency washing machines.
PCTTS 466: 20XX
3
1 Scope
This national standard provides the specification for synthetic laundry detergent powder, herein referred to as detergent. It specifies the chemical and physical requirements identifying maximum and minimum permissible limits of key parameters. It also covers essential ingredients, test methods and requirements for packaging, labelling and sampling.
This national standard is applicable to synthetic laundry detergent powder intended primarily for washing household textile products using conventional washing machines, or by manual means.
This national standard does not apply to liquid laundry detergent.
This national standard does not include methods for measuring the performance of synthetic laundry detergent powder.
2 Normative references
The following referenced documents are indispensable for the application of this standard. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
ASTM International
ASTM D 502-89 (Reapproved 2003), Standard test method for particle size of soaps and other detergents
ASTM D 2667-89 (Reapproved 2008), Standard test method for biodegradability of alkylbenzene sulphonates
British Standards Institution
BS 1647: Part 1: 1984, pH Measurement – Part 1. Specification for pH scale
BS 1647: Part 2: 1984, pH Measurement – Part 2. Specification for reference value standard solutions and operational reference standard solutions
BS 3145: 1978, Specification for laboratory pH meters
BS 3762: Section 3.15: 1985, Analysis of formulated detergents – Part 3. Quantitative test methods – Section 3.15 Method for estimation of carboxymethylcellulose content
BS 3762: Section 3.7: 1986, Analysis of formulated detergents – Part 3. Quantitative test methods – Section 3.7 Method for determination of total non-ionic matter content
International Organization for Standardization
ISO 2271: 1989, Surface active agents – Detergents – Determination of anionic-active matter by manual or mechanical direct two-phase titration procedure
ISO 2871-1: 1988, Surface active agents – Detergents – Determination of cationic-active matter content – Part 1 – High-molecular-mass cationic-active matter
ISO 2871-2: 1990, Surface active agents – Detergents – Determination of cationic-active matter content – Part 2: Cationic-active matter of low molecular mass (between 200 and 500)
ISO 4313: 1976, Washing powders – Determination of total phosphorous(V) oxide content - Quinoline phosphomolybdate gravimetric method
PCTTS 466: 20XX
4
ISO 8215: 1985, Surface active agents – Washing powders – Determination of total silica – Gravimetric method
Trinidad and Tobago Bureau of Standards
TTS 76: Part 15, Requirements for labelling – Labelling of general household and automotive cleaning chemicals
3 Terms and definitions
For the purposes of this national standard the following terms and definitions shall apply. 3.1 active ingredients the organic surface active material present in the detergent
NOTE Permissible types of active ingredient include anionic, cationic and non-ionic.
3.2 address the full postal address of the principal place of business or registered office of the manufacturer or distributor of the cleaning chemical
3.3 agglomeration a mass of powder particles bound loosely together into a cluster
3.4 anionic surface active agent a surface active agent which ionizes in aqueous solution to produce negatively charged organic ions which are responsible for the surface activity
3.5 anti-redeposition agent a substance that inhibits the redeposition of suspended soil in a washing bath, that was previously removed from the fabric
3.6 appropriate authority a person, officer or authority administering a law regulating the importation, manufacture or use of toxic chemicals 3.7 batch detergent of a single type, grade, class and composition manufactured under the same conditions
3.8 biodegradable capable of being decomposed into innocuous products by living matter
PCTTS 466: 20XX
5
3.9 builder a material added to the detergent formulation that enhances or maintains the cleaning efficiency of the surface active agent, principally by inactivating water hardness either by sequestration, precipitation or ion exchange
NOTE Secondary benefits may include supplying alkalinity, buffering to maintain alkalinity at optimum effective cleaning levels, adding anti-redeposition properties and emulsifying oily soil.
3.10 cationic surface active agent a surface active agent which ionizes in aqueous solution to produce positively charged organic ions which are responsible for the surface activity
3.11 defect a non-conformance with a requirement of the standard
3.12 defective unacceptable or unsuitable for distribution or sale as determined by conformity with this national standard
3.13 detergent a composition that removes soil
3.14 distributor the person or organisation actually engaged in the marketing of synthetic laundry detergent powder
NOTE The manufacturer may be its own distributor.
3.15 foreign matter matter not intended to be part of the detergent composition by the manufacturer
3.16 homogenous having a uniform structure and composition
3.17 laundry detergent powder a substance primarily intended for the wet-cleaning of household textile products, which contains a surfactant as an essential component for laundering fabrics
3.18 lot all the packages in a consignment containing material of the same grade and drawn from the same batch
PCTTS 466: 20XX
6
3.19 manufacturer the person or organization actually engaged in or principally responsible for manufacturing or producing the laundry detergent
3.20 mixed active ingredient detergent a detergent containing a mixture of surface active agents
3.21 moisture and volatile matter water and other materials in a detergent that are volatile under the conditions of the test
NOTE This test is detailed in Annex A.
3.22 non-ionic surface active agent a surface active agent which does not produce ions in an aqueous solution, but has functional groups which are responsible for its surface activity
3.23 primary package the unit in which the detergent is stored, which is labelled, and distributed for individual sale
EXAMPLE It may be a carton, sachet, box or bag.
3.24 secondary package a parcel consisting of primary packages of detergents, grouped together for ease of handling, transport, distribution or sale
3.25 soil matter out of place, on the fabric, that is to be removed by the detergent
3.26 surface active agent surfactant a material which when added to a liquid medium, modifies the properties of the medium at a surface or interface
4 Requirements
4.1 General requirements
4.1.1 Physical appearance
4.1.1.1 The detergent shall be homogenous in appearance and shall consist of non-segregating, free-flowing powder.
PCTTS 466: 20XX
7
4.1.1.2 In the instance that caking or lumping occurs during normal storage, agglomerations must be capable of easy dispersal with little manual effort.
4.1.1.3 The detergent shall be visibly free from foreign matter.
4.1.2 Dispersibility
The detergent shall be readily dispersible in water.
4.1.3 Effect on health
The manufacturer, importer and distributor of the finished product shall be able to provide evidence that the product, when used in accordance with the stipulated directions, shall not cause any harm or threat to human health or the environment.
NOTE When washing by manual means, suitable protective measures should be taken against the detergent’s typically drying nature. Further, persons bearing special topical sensitivity to detergents should also take the necessary precautions.
4.1.4 Contents
The net weight of the contents of the package shall not be less than that stated on the label as determined in accordance with Annex E.
4.2 Specific requirements
4.2.1 Storage properties The detergent shall meet the requirements stated in clauses 4.1.1 to 4.1.4, for a period of at least twelve (12) months from the date of manufacture, when stored according to the manufacturer’s instructions.
4.2.2 Ingredients
4.2.2.1 The detergent shall contain the following as essential components:
a) surface active agents;
b) builders; and
c) anti-redeposition agents.
4.2.2.2 The detergent shall meet the requirements for biodegradability as specified in Table 1.
NOTE The detergent may also contain special purpose additives to enhance performance, convenience, or product appeal. A list of commonly used ingredients is presented in Annex F.
4.2.2.3 The detergent shall not contain any ingredient which poses a threat to human health or the environment or is deemed unsuitable for use by the appropriate authority.
NOTE For ingredients not known as suitable surfactants, builders or additives for laundry detergents, the manufacturer or distributor should provide evidence that such substances have been found to be harmless to human health and the environment and suitable for use as such.
PCTTS 466: 20XX
8
4.2.3 Chemical and physical requirements
The detergent’s properties shall comply with the requirements presented in Table 1 when analysed according to test methods specified for each property.
Table 1 — Chemical and physical requirements
Property Limit Test Method
Minimum Maximum
Moisture and volatile matter content at 105 °C max. (wt %) - 15 Annex A
pH of 1 % aqueous solution at 27 °C 9.0 11.0 Annex B
Water insoluble matter (wt %) - 5.0 Annex C
Free alkali as NaOH (wt %) - 0.1 Annex D
Anionic active ingredient (wt %) a 12 - ISO 2271: 1989
Total mixed active ingredient detergent b 12 -
- anionic active ingredient (wt %) 8 - ISO 2271: 1989
- other active ingredient c (wt %) 1.5 -
(ISO 2871-1: 1988 and ISO 2871-2: 1990) d and/or BS 3762-3.7:
Sodium carboxymethylcellulose (wt %) f 0.2 - BS 3762-3.15: 1985
Biodegradability of alkylbenzene sulphonate (where applicable) (% surfactant reduction)
80 - ASTM D 2667-89
Particle size
Material passing through a US standard #10 (2000 µm) sieve (wt %)
100
-
Material passing through a US standard #200 (75 µm) sieve (wt %)
- 3
Procedure as detailed in ASTM D 502-89 except
use US #10 and US #200 standard sieves
a This applies if only anionic surfactants are used. b The minimum amounts of anionic and other active ingredients are specified, and add up to 9.5 %. The total minimum amount
of mixed active ingredient shall be 12 %, the remaining 2.5 % being either anionic or other active ingredient. c Other active ingredients are cationic and/or non-ionic active ingredient. d The total cationic active ingredient (wt %) is equal to the sum total of the cationic active ingredient value (wt %) obtained from
both ISO 2871-1: 1989 and ISO 2871-2: 1989. e BS 3762-3.7:1986 is used to determine the wt % for non-ionic active ingredient only. f This applies if sodium carboxymethylcellulose is the only anti-redeposition agent used.
PCTTS 466: 20XX
9
5 Test methods
Tests for compliance with the specified limits for properties listed in Table 1 shall be carried out in accordance with the method specified for each property in Table 1. Compliance with the requirement specified in clause 4.1.4 shall be determined by the test method described in Annex E.
6 Sampling
6.1 Sample size
Each lot shall be tested separately for compliance with the requirements of this standard. The number (n) of primary packages to be selected to constitute a representative sample of the lot shall depend on the size of the lot (N). The sample size for each lot shall be in accordance with Table 2.
Table 2 — Scale of sampling
Lot or batch size, N
(# of primary packages)
Sample size, n
(# of primary packages)
2 - 25 2
26 - 150 3
151 - 1200 5
1201 - 35000 8
35001 and over 13
NOTE The sample and lot sizes above were determined using Tables 1 and 2-A of ISO 2859-1:1999 – Sampling procedures by attributes - Part 1: Sampling schemes indexed by acceptance quality limit (AQL) for lot-by-lot inspection. This applies to a single sampling plan for normal inspection and a special inspection level of S-2.
6.2 Selection of primary packages
The primary packages shall be selected systematically as described in 6.2.1 or randomly using random number tables. 6.2.1 Starting from any package, count and number all the primary packages in numerical order as 1, 2, 3, 4 …… up to r (defined below), and withdraw every rth package thus counted to give a sample for the test.
Where r = integral part of N/n N = the lot or batch size n = the number of primary packages to be selected (sample size) 6.2.2 Where primary packages are grouped into secondary packages, as far as it is possible, only one package from each outer case shall be selected until the entire sample has been collected. Every effort shall be made to collect sample primary packages representative of all packing positions in the
PCTTS 466: 20XX
10
secondary packages. The selection of secondary packages for the sampling exercise shall be carried out in accordance with 6.3.
6.3 Selection of secondary packages
6.3.1 Where the number of secondary packages exceeds the sample size (n), secondary packages will be selected randomly for inclusion in the sampling exercise.
6.3.2 Where the sample size (n) exceeds the number of secondary packages, every effort shall be made to apportion sampling quotas equally among the secondary packages of the lot.
7 Conformity to requirements
7.1 Lot conformity
The entire lot shall be deemed as conforming to the requirements of this standard when the samples taken in accordance with clauses 6.2 and 6.3 conform to the chemical and physical requirements specified in Table 1. 7.2 Conformity assessment
7.2.1 For each property to be tested on the individual samples of the lot, the mean ( x ) value and the range (R) value shall be calculated as follows:
Mean ( x ) = Sum of test results Number of primary packages sampled Range (R) = The difference between the maximum and minimum values of the test results 7.2.2 The samples shall be deemed as conforming to a particular chemical or physical requirement under the following conditions:
a) if the value of the expression ( Rx 4.0− ) is greater than or equal to the minimum value specified for the property in Table 1, for which only the minimum value is given; b) if the value of the expression ( Rx 4.0+ ) is less than or equal to the maximum value given specified for the property in Table 1, for which only the maximum value is given; or c) if the value of the expression ( Rx 4.0± ) falls within the range of values specified for the property in Table 1, for which both the maximum and minimum values are given.
PCTTS 466: 20XX
11
8 Packaging and labelling
8.1 The detergent shall be packed in securely closed packages to ensure that the performance of the detergent is not affected and to prevent leakage.
8.2 Packages for individual sale shall be conspicuously and legibly labelled and/or marked to convey the following information:
a) the name of the product which includes the words "laundry," "detergent," and "powder" or "powdered";
EXAMPLE The name may be "powdered laundry detergent" or "laundry detergent powder".
b) the brand name of the product and/or recognized trade mark, where applicable;
c) the name and address of the manufacturer and/or distributor;
d) the country of origin;
e) the net weight of the contents of the packaged product in SI units;
f) instructions for applicable usage;
g) precautions for use or potential hazards presented by product use;
h) the month and year of manufacture;
i) a "best before" date;
j) the batch number or lot number stated in code or otherwise; and
k) a caution statement as to the irritant capability of the detergent.
EXAMPLE Detergent solution can be a skin irritant. Avoid prolonged contact. Rinse garment and hands thoroughly.
l) first aid instructions, in the event of contact, inhalation, absorption, ingestion, fire, spillage or leakage of packages.
NOTE Where the product has been certified by the Trinidad & Tobago Bureau of Standards, it may also bear the TTBS standard mark.
8.3 Labelling shall also comply with the requirements of TTS 76: Part 15, Requirements for Labelling – Labelling of general household and automotive cleaning chemicals.
PCTTS 466: 20XX
12
Annex A (normative)
Determination of moisture and volatile matter content
A.1 Apparatus
a) Desiccators
b) Oven capable of maintaining 105 °C
c) Petri dish
d) Analytical balance (accuracy of ± 0.05 g)
A.2 Procedure
a) Weigh 10 g ± 0.1 g of detergent into a previously weighed Petri dish.
b) Dry in an oven at 105 °C ± 5 °C for two hours.
c) Cool in a desiccator and weigh.
d) Continue heating, cooling and weighing until a constant weight is obtained.
A.3 Calculation
% moisture and volatile matter in sample = 100 x m/M
Where m = mass of Petri dish & original sample – mass of Petri dish & dried sample
M = mass of original sample
PCTTS 466: 20XX
13
Annex B (normative)
Determination of pH value
B.1 Apparatus
a) pH meter: A standard pH meter which meets the requirements of BS 3145: 1978, Specification for laboratory pH meters
b) Volumetric flask: 1000 ml capacity
c) Beaker: 100 ml capacity
d) Analytical balance (accuracy of ± 0.0005 g)
B.2 Reagents
a) Distilled water
b) Standard buffer solution: Any suitable buffer solutions within the pH range of 9 to 11 units for calibrating the pH meter
B.3 Procedure
a) Ensure that the pH meter is calibrated with standard buffer solutions before use (see also parts 1 & 2 of BS 1647, pH measurement).
b) Weigh 10 g ± 0.001 g of the material and transfer to a 1 L volumetric flask.
c) Partially fill the flask with distilled water, stopper tightly and agitate until the sample is completely dissolved.
d) Adjust the temperature of the solution and the distilled water to 27 °C ± 0.5 °C, and fill to the calibration mark with the distilled water.
e) Stopper the flask, mix thoroughly and allow the solution to stand at a temperature of 27 °C for two hours prior to reading the pH value.
PCTTS 466: 20XX
14
Annex C (normative)
Determination of matter insoluble in water
C.1 Apparatus
a) Desiccator
b) Beaker, capacity 250 ml
c) Steam bath
d) Buchner crucible
e) Erlenmeyer filter flask
f) Watch glass
g) Oven capable of maintaining 105 °C ± 5 °C
h) Analytical balance (accuracy of ± 0.005 g)
C.2 Reagent
Ethyl alcohol – Freshly boiled, reagent grade, 95 % or higher, neutral to phenolphthalein
C.3 Procedure
a) Weigh 2 g to 10 g ± 0.01 g of the sample into a 250 ml beaker.
b) Digest the sample with 200 ml of freshly boiled ethyl alcohol in a covered vessel on a steam bath until the soap is dissolved.
c) Filter through a weighed Buchner crucible with suction, protecting the solution from carbon dioxide and other acid fumes during the operation by covering with a watch glass.
d) Wash the residue in the crucible with hot neutral ethyl alcohol until free from soap. Reserve the filtrate and washings.
e) After filtering and thoroughly washing the residue, change the receiver. Extract the residue with water at 100 °C and wash the residue thoroughly.
f) Dry the crucible and residue at 100 °C to 105 °C for three hours. Cool and weigh the matter insoluble in water.
PCTTS 466: 20XX
15
C.4 Calculation
Matter insoluble in water, percent by mass = 100 x m/M
Where m = mass in g of dried Buchner crucible & residue – mass in g of empty Buchner crucible
M = mass in g of the sample taken for the test.
PCTTS 466: 20XX
16
Annex D (normative)
Determination of free alkali as NaOH
D.1 Apparatus
a) Bunsen burner or hot plate
b) Erlenmeyer flask
c) Burette
d) Analytical balance (accuracy of ± 0.005 g)
D.2 Reagents
a) Phenolphthalein indicator 1 % solution
b) Hydrochloric acid standard 0.1 N
D.3 Procedure
a) Heat the reserved filtrate and washings to incipient boiling [see clause c.3 (d)].
b) Add 0.5 ml of a 1 % solution of phenolphthalein.
c) Titrate with standard 0.1 N HCl solution and calculate the free alkali as sodium hydroxide (NaOH).
D.4 Calculation
Free alkali as NaOH (% by mass) = 40 x 0.1 V x 100 M
Where V = volume in ml of HCl used in titration
M = mass in g of the sample taken for the test (from annex C).
PCTTS 466: 20XX
17
Annex E (normative)
Determination of net weight of product
E.1 Apparatus
a) Top-loading balance (accurate to ± 0.05 g)
b) Container capable of holding the contents of the package of detergent
E.2 Procedure
a) Weigh the empty container.
b) Empty as much of the contents of the package into the container and record the weight.
E.3 Calculation
The average of the difference in weight shall be taken as the net weight per package.
Net weight = mass in g of container & contents – mass in g of empty container
PCTTS 466: 20XX
18
Annex F (informative)
Additional commonly used detergent ingredients
The following is a list of additional commonly used detergent ingredients:
a) Corrosion inhibitors
b) Fluorescent whitening agents
c) Processing aids
d) Colorants
e) Fragrances
f) Oxygen bleach
g) Enzymes
h) Suds control agents
i) Fabric softening agents
j) Other ingredients which provide specialized performance or convenience
