JPH0510871A - Standard sample and method for measuring ASTM color of petroleum products using the sample - Google Patents

Abstract

(57) [Summary] [PROBLEMS] To provide a standard sample used for measuring an ASTM color using a colorimeter and a method for measuring an instrument using the standard sample. [Structure] 3-methyl-1-phenyl-4- (phenylazo) -pyrazol-5-ol, 1- (phenylazo) -2-naphthalenol, 1-[[4-[(dimethylphenyl) azo] dimethylphenyl] azo ] -2-Naphthalenol, 1,5 (or 1,8) -bis [(4-methylphenyl) amino] -9,10-anthracenedione, 1-hydroxy-4-[(4-methylphenyl) amino]- 9,10-anthracenedione, 1,4-bis (butylamino) -9,10-anthracenedione and 1,4-bis [(4-butylphenyl) amino]-
It consists of a mixed solution containing 5,8-dihydroxy-9,10-anthracenedione as a colorant, 1-phenyl-1-xylylethane as a colorant solvent and dodecane as a diluent. A standard sample used for instrumental measurement with a meter, and a measurement method using the sample.

Description

Detailed Description of the Invention

[0001]

FIELD OF THE INVENTION The present invention relates to a standard sample used for measuring the ASTM color by a color difference meter, which is a color test method for petroleum products such as various lubricating oils, petrolatum and microcrystalline wax, and the standard sample. The present invention relates to a method for measuring the ASTM color of a petroleum product using a device.

[0002]

2. Description of the Related Art As a petroleum product color test method, JIS K
There are two test methods, ASTM color and Saybolt color, defined in 2580.

Among them, the ASTM color test method is a test method applied to various lubricating oils, petrolatum and the like, and this method is generally a test sample obtained by comparing with standard color glass using an ASTM color tester. This is a method of representing a color by a code of 0.5 (light) to 8.0 (dark). The standard color glass used here is XYZ of JIS Z 8722.
The variation is defined by the luminous transmittance using the color system and the standard light C and the chromaticity coordinates by the RGB color system.

[0004]

DISCLOSURE OF THE INVENTION Problems to be Solved by the Invention
When the M color tester is used, the ASTM color is judged by human vision, and the display result of the measurement method is not quantitative (when the sample color is between two standard colored glasses, Add L to the code of the darker standard color glass, or D8.0 if the sample color is darker than 8.0.
Therefore, it is the actual situation that the measurer is having difficulty in making a judgment because individual differences tend to occur. Especially when the color is dark or dark, this tendency is remarkable.

Therefore, at present, even in such a test method, there is a demand for automation instead of a visual method.

Therefore, the present inventors tried to examine whether or not this ASTM color can be measured using a commercially available colorimeter (measuring instrument).

The color difference meter uses ASTM color 0.5 to 8.0.
In all areas, the test method specified in JIS K 2580 must be well correlated. Furthermore, a universal method is desired as a test method for object color, especially liquid color.

Further, the amount of stimulus of the three primary colors of light, red, green and blue, is important for the perception of color that the human eye feels under natural light.
To measure color with an optical instrument, natural light is the light source and the stimulus amount is the tristimulus value.

Therefore, the ASTM color test method is as follows:
A universal method close to human perception based on tristimulus values by optical instruments, and a measurement result display method is L display,
Quantitative display that does not use D display is desirable. for that reason,
Recommended by the International Commission on Illumination (CIE), JIS Z 87
There is a demand for a quantitative measurement result display method based on the test method based on the object color measurement method specified in No. 22 and the color display method based on the XYZ color system specified in JIS Z 8701.

When a color is measured by a colorimeter, it is necessary to convert a measurement instruction value obtained by a commercially available colorimeter for a sample into an ASTM color. Therefore, it is necessary to find the correlation between the two.

The present inventors have compared the sum ΣD of optical densities based on the XYZ color system of standard color glass with the ASTM color, and have found that there is a correlation between the two.

That is, the relationship is expressed by the following equation.

A = αΣD + β [where A is the ASTM color and ΣD is the sum of the optical densities (DX +
DY + DZ), α and β are constants for instrumental error correction] Therefore,
By measuring the measured values X, Y, Z on the basis of the above relational expression in the calculation and display section of the measuring instrument, the measured value of the ASTM color is obtained.

Since the above-mentioned ΣD changes for each device due to the instrumental difference of the device used, it does not become the same value for the same sample. Therefore, it is necessary to prepare an ASTM color liquid standard sample and to use it to calibrate each device (colorimeter).

Such a standard sample is required to have a low volatility of the base material, be hard to be oxidized, have little deterioration with time such as oxidation, and have good color stability.

The present invention has been made based on such a viewpoint, and an object thereof is to provide a standard sample used when measuring an ASTM color by using a colorimeter and a device measuring method using the sample. To do.

[0017]

Means for Solving the Problems The inventors of the present invention have conducted a study in accordance with the above-mentioned object, and as a result, searched for a mixed colorant (dye) satisfying such requirements and found that a mixed colorant was dissolved in a specific solvent. It was found that the hue was in agreement with the standard color glass used in the ASTM color test method, and it was sufficiently effective as a standard sample.

That is, the present invention provides 3-methyl-1-phenyl-4- (phenylazo) -pyrazol-5-ol, 1- (phenylazo) -2-naphthalenol, 1-
[[4-[(Dimethylphenyl) azo] dimethylphenyl] azo] -2-naphthalenol, 1,5 (or 1,
8) -bis [(4-methylphenyl) amino] -9,1
0-anthracenedione, 1-hydroxy-4-[(4
-Methylphenyl) amino] -9,10-anthracenedione, 1,4-bis (butylamino) -9,10-anthracenedione and 1,4-bis [(4-butylphenyl) amino] -5,8- Dihydroxy-9,10-
AS for petroleum products, which comprises a mixed solution of anthracenedione as a colorant, 1-phenyl-1-xylylethane as a colorant solvent and dodecane as a diluent, respectively.
A standard sample used for instrumental measurement of TM color with a colorimeter.

According to the present invention, the ASTM of petroleum products is characterized in that a color difference meter is calibrated with the standard sample.
A method for measuring a color device is provided.

Each colorant used in the present invention has the following chemical structural formula.

(1) 3-Methyl-1-phenyl-4-
(Phenylazo) -pyrazol-5-ol (3-meth
yl-1-phenyl-4- (phenylazo) -pyrazol-5-ol)

[0022]

[Chemical 1] (CAS No. 4314-14-1) Color Index (CI): Solvent Yellow 16 For example, Oil Yellow 5GS Extra (trade name) can be mentioned.

(2) 1- (phenylazo) -2-naphthalenol

[0024]

[Chemical 2] (CAS No.842-07-9) Color Index (CI): Solvent Yellow 14 For example, Oil Orange Extra (trade name) can be mentioned.

(3) 1-[[4-[(dimethylphenyl) azo] dimethylphenyl] azo] -2-naphthalenol (1-[[4-[(dimethylphenyl) azo] dimethylpheny
l] azo] -2-naphthalenol)

[0026]

[Chemical 3] (CAS No. 1320-06-5) Color Index (CI): Solvent Red 27 For example, Oil Red 5B Special (trade name) can be mentioned.

(4) 1,5 (or 1,8) -bis [(4-methylphenyl) amino] -9,10-anthracenedione (1,5 (or1,8) -bis [(4-methylph
enyl) amino] -9,10-anthracenedione)

[0028]

[Chemical 4] (CAS No. 8005-40-1) Color Index (CI): Solvent Violet
14 For example, Oil Violet 3R (trade name) can be mentioned.

(5) 1-hydroxy-4-[(4-methylphenyl) amino] -9,10-anthracenedione (1-hydroxy-4-[(4-methylphenyl) amino] -9,
10-anthracenedione)

[0030]

[Chemical 5] (CAS No. 81-48-1) Color Index (CI): Solvent Violet
13 Examples include Oil Violet B-2R (trade name).

(6) 1,4-bis (butylamino)-
9,10-Anthracenedione (1,4-bis (butylami
no) -9,10-anthracenedione)

[0032]

[Chemical 6] (CAS No. 17354-14-2) Color Index (CI): Solvent Blue 35 For example, Oil Blue SB (trade name) can be mentioned.

(7) 1,4-bis [(4-butylphenyl) amino] -5,8-dihydroxy-9,10-anthracenedione (1,4-bis [(4-butylphenyl) amin]
o] -5,8-dihydroxy-9,10-anthracenedione)

[0034]

[Chemical 7] (CAS No. 28198-05-2) Color Index (CI): Solvent Green 28 For example, Oil Green SG (trade name) can be mentioned.

Mixing ratio (volume ratio) of these 7 colorants
Is (1) :( 2) :( 3) :( 4) :( 5) :( 6) :( 7) = 18
It is particularly desirable that the ratio is 3: 53: 13: 11: 16: 1: 3.

Further, in the present invention, 1 is used as the solvent for the colorant.
-Phenyl-1-xylylethane (1-phenyl-1-xylylet
hane, hereinafter referred to as PXE) and dodecane (hereinafter referred to as nC ₁₂ ) as a diluent, respectively.

The preparation of a specific standard sample will be described.
First, predetermined amounts of the above 7 kinds of colorants were separately dissolved in a PXE solvent to obtain 1000 ppm (wt / vol) of each.
%) Diluted solution. Then, the mixture of these seven dilutions with mixing ratio of the (volume ratio), further a predetermined amount and diluted with n-C ₁₂ a predetermined dilution ratio of the mixed solution (e.g., 2-350 times) Prepare a standard sample.

Next, the device measuring method of the present invention will be described.

The above standard sample (for example, true ASTM color =
Assuming that the ASTM color of 7.0) is 6.98 when measured by the color difference meter based on the sum (ΣD) of the optical densities of the sample and the previously determined relational expression, the calculation is performed. , Calibrate the colorimeter by setting the value to 7.0 using the correction key on the display.

This calibration (correction) is performed using true ASTM color 0.
By using the respective standard samples of 5 to 8.0 and calibrating the colorimeter, the colorimeter can be used accurately.

As described above, by using the standard sample of the present invention, the instrumental measurement of the ASTM color of petroleum products can be quantitatively and accurately performed.

[0042]

EXAMPLES The present invention will be specifically described below based on examples.

Example 3-Methyl-1-phenyl-4- (phenylazo)-
Pyrazol-5-ol, 1- (phenylazo) -2
-Naphthalenol, 1-[[4-[(dimethylphenyl) azo] dimethylphenyl] azo] -2-naphthalenol, 1,5 (or 1,8) -bis [(4-methylphenyl) amino] -9,10 -Anthracenedione,
1-Hydroxy-4-[(4-methylphenyl) amino] -9,10-anthracenedione, 1,4-bis (butylamino) -9,10-anthracenedione, and 1,4-bis [(4- Butylphenyl) amino]
Predetermined amounts of seven colorants of -5,8-dihydroxy-9,10-anthracenedione were separately added to 1-phenyl-1-
Dissolve in xylyl ethane solvent, each 1000p
Make a diluted solution of pm (wt / vol%). Next, these seven diluted solutions were added to ::::::: = 18
Ratio of 3: 53: 13: 11: 16: 1: 3 (capacity ratio)
Then, a predetermined amount of this mixed solution was diluted with n-C12 to prepare 31 kinds of standard samples having the dilution ratio shown in Table 1.

Sum of optical densities of the above standard samples (ΣD)
Was measured using a color difference meter (Chroma meter CT-210custom, manufactured by Minolta Camera Co., Ltd.) with a sampling cell having a cell length of 33 mm and using a standard C light source (CIE standard source C). Furthermore, the AS of each standard sample
The TM color was measured by four measurers (A to D) using a conventional ASTM color tester. The results are shown in Table 1 and FIG. 1, respectively.

[0045]

[Table 1] As shown in Table 1 and FIG. 1, the sum (ΣD) of the optical densities of the respective standard samples preferably corresponds to the respective ASTM colors. Further, the repetitive error of ΣD was small.

[0046]

As described above, by using the standard sample of the present invention, the instrumental measurement of the ASTM color of petroleum products can be quantitatively and accurately performed.

[Brief description of drawings]

FIG. 1 is a graph showing the relationship between ΣD and ASTM color.

Claims (4)

[Claims] 1. 3-Methyl-1-phenyl-4- (phenylazo) -pyrazol-5-ol, 1- (phenylazo) -2-naphthalenol, 1-[[4-[(dimethylphenyl) azo] dimethylphenyl ] Azo] -2-naphthalenol, 1,5 (or 1,8) -bis [(4-
Methylphenyl) amino] -9,10-anthracenedione, 1-hydroxy-4-[(4-methylphenyl)
Amino] -9,10-anthracenedione, 1,4-bis (butylamino) -9,10-anthracenedione and 1,4-bis [(4-butylphenyl) amino]-
It consists of a mixed solution containing 5,8-dihydroxy-9,10-anthracenedione as a colorant, 1-phenyl-1-xylylethane as a colorant solvent and dodecane as a diluent. A standard sample used when measuring equipment with a meter. 2. The 3-methyl-1-phenyl-4-
(Phenylazo) -pyrazol-5-ol, 1- (phenylazo) -2-naphthalenol, 1-[[4-
[(Dimethylphenyl) azo] dimethylphenyl] azo] -2-naphthalenol, 1,5 (or 1,8)-
Bis [(4-methylphenyl) amino] -9,10-anthracenedione, 1-hydroxy-4-[(4-methylphenyl) amino] -9,10-anthracenedione, 1,4-bis (butylamino) The compounding ratio (volume ratio) of -9,10-anthracenedione and 1,4-bis [(4-butylphenyl) amino] -5,8-dihydroxy-9,10-anthracenedione was 18 each.
3: 53: 13: 11: 16: 1: 3.
The standard sample described in. 3. 3-Methyl-1-phenyl-4- (phenylazo) -pyrazol-5-ol, 1- (phenylazo) -2-naphthalenol, 1-[[4-[(dimethylphenyl) azo] dimethylphenyl ] Azo] -2-naphthalenol, 1,5 (or 1,8) -bis [(4-
Methylphenyl) amino] -9,10-anthracenedione, 1-hydroxy-4-[(4-methylphenyl)
Amino] -9,10-anthracenedione, 1,4-bis (butylamino) -9,10-anthracenedione and 1,4-bis [(4-butylphenyl) amino]-
Calibrate the colorimeter with a standard sample consisting of a mixed solution containing 5,8-dihydroxy-9,10-anthracenedione as a colorant, 1-phenyl-1-xylylethane as a colorant solvent and dodecane as a diluent. A method for measuring the ASTM color of petroleum products, which is characterized in that 4. The 3-methyl-1-phenyl-4-
(Phenylazo) -pyrazol-5-ol, 1- (phenylazo) -2-naphthalenol, 1-[[4-
[(Dimethylphenyl) azo] dimethylphenyl] azo] -2-naphthalenol, 1,5 (or 1,8)-
Bis [(4-methylphenyl) amino] -9,10-anthracenedione, 1-hydroxy-4-[(4-methylphenyl) amino] -9,10-anthracenedione, 1,4-bis (butylamino) The compounding ratio (volume ratio) of -9,10-anthracenedione and 1,4-bis [(4-butylphenyl) amino] -5,8-dihydroxy-9,10-anthracenedione was 18 each.
3: 53: 13: 11: 16: 1: 3.
The method described in.