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SEMI C1-0705 © SEMI 1978, 2005 4 4.19.1 Where feasible, a specification of c ont ent shall be expressed as a numerical limit in units of weight by weight. For a specification that canno t be assigned such a limit , the e…
SEMI C1-0705 © SEMI 1978, 2005 3
4.10 Drying or Igniting to Constant Weight — A statement “dried to a constant weight” or “ignited to a constant
weight” shall imply that two separate weighings differ by no more than ± 0.4 mg (unless otherwise specified), where
the second weighing follows a second drying (for one hour (unless otherwise stated) or ignition for 15 minutes
(unless otherwise stated), respectively.
4.11 Expression of Content and Concentration — Unless otherwise stated, a specification limit and experimental
results related to it shall be expressed in units of weight by weight. The concentration of a solution of a test reagent
shall be expressed either in molarity or normality or as percent weight by volume. A redox normality value shall
always be followed, parenthetically, by the relevant molarity. In the approximate dilution of reagents, a
parenthetical expression of two numbers with an intervening “plus” sign shall imply that the relative volume of the
stated reagent given by the first number shall be admixed with the relative volume of water given by the second
number. Thus, “dilute” sulfuric acid (1 + 3) directs that one volume of reagent grade sulfuric acid be added to 3
volumes of water and the mixture stirred to form a uniform solution.
4.12 Filtration — A statement to “filter,” unless qualified, shall imply filtration through suitable filter paper until
the filtrate is clear.
4.13 Physical Properties — Physical properties shall not usually be employed for specification purposes; for
information, however, representative values for a particular liquid chemical, as supplied, may be included in the
standard for that liquid chemical. Where relevant, physical properties shall be specified for 25°C.
4.14 Reagent Chemicals — Unless otherwise stated, reagents to be used in tests shall conform to the minimum
standards of quality set forth in the current edition of Reagent Chemicals, published by the American Chemical
Society
5
.
4.15 Residue after Evaporation — A “residue after evaporation” test may be used in the assessment of liquid
chemicals. (See Determination of Residue after Evaporation, ¶7.4.)
4.16 Residue after Ignition — A “residue after ignition” test serves to assess the amount of nonvolatile inorganic
matter present in a sample. (See Determination of Residue after Ignition, ¶7.5.)
4.17 Rounding of Numbers — The following rules for “rounding” of measured or calculated values shall be
employed:
4.17.1 When the figure next beyond the last place to be retained is less than 5, leave unchanged the figure in the last
place retained.
4.17.2 When the figure next beyond the last place to be retained is greater than 5, increase by 1 the figure in the last
place retained.
4.17.3 When the figure next beyond the last place to be retained is 5 and there are no figures beyond this 5 or only
zeroes, (a) increase by 1 the figure in the last place retained if it is odd, or leave the figure unchanged if it is even.
4.17.4 When the figure next beyond the last place to be retained is 5 and there are figures other than zeroes beyond
this 5 increase by 1 the figure in the last place retained.
4.17.5 Obtain the rounded value in one step by direct rounding and not in two or more steps of successive
roundings.
4.18 Samples and Sampling — For liquid chemicals provided in small containers, one (or more) should be freshly
opened for testing, thereby reducing possibilities for contamination or change in composition (for example, by
moisture pickup). Where the liquid chemical is provided in larger bulk quantities, one or more drums or other
containers shall be sampled to avoid cross contamination, and the combined sample shall be placed in a labeled,
well-cleaned container that shall be tightly closed and transferred expeditiously to the testing laboratory.
4.19 Specifications and Specification Limits — The specifications provided by this guide are intended to serve for
liquid chemicals to be used in the manufacture and processing of semiconductors and advanced electronic devices
and circuits. The specifications and the associated test procedures are based on the experience of suppliers and users
and also on published studies relating to liquid chemicals of the required quality. The function of the specifications
is to establish minimum standards of quality.
5 Available from American Chemical Society, 1155 Sixteenth Street, NW, Washington DC, 20036, Phone: 202-872-4600, Fax: 202-872-4615,
Website: http://www.chemistry.org
SEMI C1-0705 © SEMI 1978, 2005 4
4.19.1 Where feasible, a specification of content shall be expressed as a numerical limit in units of weight by
weight. For a specification that cannot be assigned such a limit, the expression “To pass test” shall be used.
4.19.2 For a major component, the value (assay, purity, etc.) shall be expressed as a minimum permissible limit or
range. For an impurity, the value shall be expressed as a maximum permissible limit.
4.19.3 A liquid chemical conforming to the specification will commonly contain either more of the major
component than the minimum permissible limit or be within the specified range for the liquid chemicals and contain
less of each impurity (or impurities) than the maximum permissible limit. In neither case shall the liquid chemicals
be considered as of higher quality than that defined by the specification.
4.19.4 It is manifestly impossible in the specifications and procedures for a liquid chemical to consider every
impurity or contaminant that might be present. For certain applications, it is recognized that more stringent or
additional specifications and procedures might be required. The intent of these specifications and the associated
procedures is, on one hand, to assure that a liquid chemical is suitable for the common uses to which it may be put in
the manufacture and processing of semiconductor devices and, on the other hand, to be consistent with
contemporary manufacturing processes for that liquid chemical.
4.20 Specification Parameters — The statement of specification parameters for a particular liquid chemical shall
be, as far as practical.
4.20.1 Assay or other test assessing the component(s) of interest
4.20.2 Appearance or color
4.20.3 Acidity or alkalinity, or both, or pH range of solution
4.20.4 Residue after evaporation or ignition
4.20.5 Water content
4.20.6 Diverse general tests, arranged alphabetically
4.20.7 Tests for stated anions and ammonium shall be arranged alphabetically (ammonium, chloride, nitrate,
phosphate, sulfate)
4.20.8 Tests for specific trace metals, arranged alphabetically by name. The 21 metals for grade specifications
higher than Grade 2 are Aluminum, Antimony, Arsenic, Barium, Boron, Cadmium, Calcium, Chromium, Copper,
Iron, Lead, Lithium, Magnesium, Manganese, Nickel, Potassium, Sodium, Tin, Titanium, Vanadium, and Zinc.
4.20.9 All major words in a specification parameter shall have their initial letters capitalized.
4.20.10 Following the statement of a specification parameter, where relevant, the species on which the calculation
of the result is based shall be expressed parenthetically as the atomic symbol or empirical formula.
4.21 Tared Containers — Where the use of a tared container is specified, it shall be carried through operations
identical to those used in the test procedures, including drying or ignition, or both, cooling in a desiccator, and
weighing. When a new container is placed in service, special measures may be required to assure that it is brought
to constant weight by the operations.
4.22 Temperature — Temperature values shall be expressed in degrees Celsius (°C).
4.23 Water — References to water in the testing procedures are understood to mean water that is of the appropriate
grade for the intended purpose. Depending on the grade of liquid chemical being tested, water meeting the
requirements for Types E-1, E-1.1, and E-1.2 water in ASTM Standard Guide D5127 may be used. In tests for
nitrogen compounds, water should be “ammonia-free” or “nitrogen-free.” For some tests, freshly boiled water must
be used in order to ensure freedom from material absorbed from the air such as ammonia, carbon dioxide, or
oxygen.
SEMI C1-0705 © SEMI 1978, 2005 5
4.24 Water Content by Karl Fischer Titration — The Karl Fischer method for the determination of water involves a
titration with the so-called Karl Fischer reagent, consisting of iodine, sulfur dioxide, pyridine, and methanol. Details
of this method are provided in the ASTM Standard Test Method E 203 and in Reagent Chemicals, published by the
American Chemical Society
4.25 Water and Steam Baths — A water bath, unless otherwise stated, shall imply a bath of vigorously boiling
water. A steam bath (at 1 atmosphere pressure), unless otherwise qualified, shall imply either exposure to flowing
steam or to another source of heat at the temperature of flowing steam.
4.26 Weights and Measures — The weights and measures used shall be those of the International System (SI)
6
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5 Reagent and Standard Solutions
5.1 The purity of reagents used in each analytical procedure should be concomitant with the grade of liquid
chemical being analyzed.
5.2 Ammonium Molybdate Reagent Solution — Dissolve 50 g of ammonium molybdate, (NH
4
)
6
Mo
7
O
24
•4H
2
O, in 1
N sulfuric acid and dilute with 1 N sulfuric acid to 1000 mL.
5.3 Ammonium Thiocyanate Reagent Solution — Dissolve 150 g of ammonium thiocyanate, NH
4
SCN, in water and
dilute with water to 500 mL.
5.4 Antimony Standard Solution — Dissolve and dilute 0.275 g of potassium antimony KSbO(C
4
H
4
O
6
)• 1/2H
2
O
with water to 1000 mL (1.0 mL = 0.1 mg of antimony (Sb)).
5.5 Arsenic Stock and Working Solution — See ¶7.6.3.1.
5.6 Barium Chloride Solution — Dissolve 60 g of barium chloride dihydrate, BaCl
2
•2H
2
O, in water and dilute with
water to 500 mL.
5.7 Boron Standard Solution — Dissolve 0.572 g of boric acid, H
3
BO
3
, in water and dilute to 1000 mL with water.
Then dilute 10 mL of this solution with water to 1000 mL (1.0 mL = 0.001 mg of boron (B)).
5.8 “Bromine Water” Reagent Solution — Add sufficient liquid bromine to water in a bottle so that undissolved
bromine remains as a separate phase when the mixture is shaken.
5.9 Brucine Sulfate Solution — Dissolve 0.6 g of brucine sulfate, (C
23
H
26
N
2
O
4
)
2
•H
2
SO
4
•7H
2
O, in dilute sulfuric
acid (2 + 1), previously cooled to room temperature, and dilute to 1000 mL with the dilute acid. The sulfuric acid
should be nitrate-free acid prepared as follows: Dilute the concentrated sulfuric acid (about 96% H
2
SO
4
) to about
80% H
2
SO
4
by adding it to water, heat to dense fumes of sulfur trioxide, and cool. Repeat the dilution and fuming
three or four times.
5.10 Carminic Acid Reagent Solution — Dissolve 0.05 g of carminic acid in 100 mL of sulfuric acid and shake until
dissolution is complete.
5.11 Chloride Standard Solution — Dissolve 0.165 g of sodium chloride, NaCl, in water and dilute with water to
100 mL. Then dilute 10 mL of this solution with water to 1000 mL (1.0 mL = 0.010 mg of chloride (Cl) ion).
5.12 Dimethylglyoxime Reagent Solution — Dissolve 1.0 g of dimethylglyoxime in 100 mL of 95% EtOH (ethanol)
reagent alcohol.
5.13 Hydrogen Sulfide Water — Immediately before use, saturate water with hydrogen sulfide gas.
5.14 Hydroxylamine Hydrochloride Reagent Solution — Dissolve 10 g of hydroxylamine hydrochloride,
NH
2
OH•HCl, in water and dilute with water to 100 mL.
5.15 Iron Standard Solution — Dissolve 0.702 g of ferric ammonium sulfate hexahydrate, Fe(NH
4
)
2
(SO
4
)
2
•6H
2
O,
in 10 mL of 10% sulfuric acid and dilute with water to 100 mL. Then to 10 mL of this solution, add 10 mL of 10%
sulfuric acid and dilute with water to 1000 mL (1.0 mL = 0.010 mg of iron (Fe) ion).
6 http://www.bipm.fr/enus/3_SI/, Bureau International des Poids et Mesures, Pavillon de Breteuil, 92312 Sèvres cedex, France, Phone: +33 1 45
07 70 70, Fax: +33 1 45 34 20 21, Website: http://www.bipm.fr/